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A HANDBOOK 

FOB 

CEMENT WORKS CHEMISTS 



CHARLES GRIFFIN AND CO. LTD. PUBLISHERS 

Second Edition, Bevised, Re-written. $4.50 net 

CALCAREOUS CEMENTS : 

Their Nature, Preparation and Uses 

With some Remarks upon Cement Testing 
By G. R. REDGRAVE, Assoc.I.C.E., and CHAS. SPACKMAN, F.C.S. 

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LONDON : CHARLES GBIFFIN AND Co. LTD. EXETEE ST. STEAND 

TO 15E HAD OF J. B. LlPPINCOTT COMPANY. PHILADELPHIA 



A HANDBOOK 

FOR 

CEMENT WORKS CHEMISTS 



BY 

FRANK B. GATEHOUSE, F.C.S. 

, 

ASSOCIATE OF THE MERCHANT VENTURERS* TECHNICAL COLLEGE, BRISTOL 

FORMERLY CHEMIST AT J. AND B. WHITE, BROS. (A.P.C.M. LTD ), 

SWANSCOMBE, KENT ; RESEARCH CHEMIST TO H. W. 

ANDERSON, ESQ., C.E. ; CHEMIST AT THE XEM 

HARTFORD CEMENT WORKS 



WITH ILLUSTRA TIO.\S 





LONDON 
CHARLES GRIFFIN AND COMPANY, LIMITED 

PHILADELPHIA : J. B. LIPPINCOTT COMPANY 
1908 

[AU rights reserved] 



THE Author \vishes to acknowledge his indebtedness 
to Messrs. H. W. Anderson, C.E., H. K. G. Bamber, 
F.C.S., J. W. Gatehouse, F.I.C., H. H. Slater, F.I.C., 
J. T. Stiff, the authors of the volumes consulted, 
and others who have materially assisted him during 
the preparation of this handbook. 

KINGSTON-ON-THAMES, 
1908. 



179721 



CONTENTS 

CHAPTER I 
INTRODUCTION 

Prologue Equivalent Solutions Chemicals and Apparatus required 
Books consulted ........ pp. 1-4 

CHAPTER II 
ANALYSIS OP RAW MATERIALS 

Sampling : Chalk or Limestone ; Moisture ; Loss on Ignition ; Silica and 
Insoluble ; Alumina and Iron Oxide ; Lime ; Volumetric Determination 
of CaO ; Lime as CaS0 4 ; Magnesia ; Sulphates ; Accurate Estimation of 
Carbon Dioxide ; Rapid Estimation of C0 2 Marls, Gault Clay, Calcareous 
Shales Clay Estimation of Iron by Means of Standard Permanganate 
and Standard Bichromate Loss on Ignition Total Sulphur Sulphur 
Present as Sulphate Alkalies Separation of Soda and Potash Soluble 
Chloride Shales, Sandstones, and Slates Natural Cement Rock- 
Slags Phosphorus and Sulphur pp. 5-37 

CHAPTER III 

CALCULATION OF PROPORTION OP RAW 
MATERIALS 

Limestones Clay, Shales, &c. Slurry : Moisture ; Fineness ; Estimation 
of CaC0 3 ; Preparation of a Standard Dry Slurry or Raw Meal ; Slater's 
Calcimeter; Bamber's Calcimeter ; To Calculate Percentage of CaC0 3 ; 
Estimation of CaC0 3 ; Loss on Ignition ; Calculated CaC0 3 Control 
and Alteration of the Raw Mixture pp. 38-55 

CHAPTER IV 

ANALYSIS OP FUEL, LUBRICANTS, WATER, 
AND KILN GASES 

Coal : Moisture; Ash; Volatile Matter : Fixed Carbon; Coke; Sulphur; Ana- 
lysis of Ash Analysis of Coke Calorific Power of Fuel Fineness 

vii 



viii CONTENTS 

Lubricants : Loss or Gain in Weight ; Specific Gravity ; Viscosity ; Flash 
Point ; Free Mineral Acids ; Free Fatty Acid ; Separation of Fatty and 
Mineral Oils Water Analysis : Collection of Samples ; Colour, Odour, 
Reaction ; Sediment and Suspended Matter ; Total Solids ; Chlorine as 
Chlorides ; Hardness, Temporary and Permanent ; Contamination : 
Standard Ammonium Chloride, Nessler's Reagent, Alkaline Perman- 
ganate, Estimation of Free Ammonia, Albuminoid Ammonia ; Estima- 
tion of Oxygen required to Oxidise Organic Matter ; Estimation of 
Nitrates + Nitrites ; Poisonous Metals ; Water Softening Gas Ana- 
lysis : Collection of Samples ; Analysis of Gases in the Hempel Appara- 
tus ; Filling the Burette ; Estimation of Carbon Dioxide, Oxygen, Carbon 
Monoxide, Nitrogen, Combustible Gases ; Analysis with the Orsat 
Apparatus ; Condition of Combustion in a Rotary Kiln . pp. 56-90 



CHAPTER V 
CEMENT ANALYSIS 

Accurate Methods Alumina and Ferric Oxide Lime Magnesia 
Alkalies Ordinary Method of Analysis for Technical Purposes 
Insoluble Residue Sulphuric Anhydride Sulphur as Sulphide Loss 
on Ignition Carbon Dioxide Rapid Method for Estimation of Lime in 
a Cement Analysis of Gypsum, Plaster, Keene's Cement, &c. 
Estimation of Caustic Lime (CaO) in Burnt Lime, &c. . pp. 91-103 

APPENDIX 

Examples of Calculations occurring during Analysis Directions for 
Making up Solutions Tables Typical Analyses Useful Data for 
Testing Room pp. 107-135 

INDICES .... ... pp. 137-142 




CHAPTER I 
INTRODUCTION 

As indicated by its title, this book is intended 
primarily for Cement Works Chemists, although it 
is hoped that it may be found of use in other 
laboratories. It has been the aim of the compiler, 
in order to keep the book within reasonable limits, 
to include only essential details of manipulation 
where this was possible without ambiguity. Each 
separate process will be found in a numbered para- 
graph, and a method once described is indicated in 
the text by that number when it has again to be 
carried out. An epitome of most of the processes 
will be found at the foot of the fuller description. 
In this way the book may be of use as a guide to 
younger and less experienced chemists, often found 
on cement works, as well as for reference purposes 
by the experienced, 

For the sake of uniformity the strengths and 
volumes of the solutions employed are stated accord- 
ing to Reddrop's system as described and followed 
by Phillips in his Engineering CJiemistry. 

A table will be found in the Appendix giving 
instructions for making all the necessary reagents 



2 CEMENT CHEMISTS 1 HANDBOOK 

and their strength in terms of E, this being 
the symbol used to denote the equivalent or 
equivalents of the reagent by weight, in grams 
per litre. These reagents need not be made with 
the same degree of accuracy as those employed in 
volumetric analysis. For fuller particulars reference 
should be made to the work mentioned. 

The following is a list of chemicals and apparatus 
required for the processes described in this hand- 
book : 

CHEMICALS REQUIRED. 

Pure hydrochloric acid. Soda lime. 

Commercial Potassium bichromate. 
Pure nitric acid. chromate. 

sulphuric acid. ferricyanide. 

acetic acid. ferrocyanide. 

hydrofluoric acid. nitrate (powder). 

Oleic acid. permanganate. 

Oxalic acid. carbonate. 

Pyrogallol. hydrate. 

Pure ammonium hydrate (-880). bisulphate. 

j> oxalate. ,, chlorate. 

?? ,, thiocyanate. Ferrous ammonium sulphate. 

Ammonium carbonate. Magnesium chloride. 
chloride. oxide. 

molybdate. Manganese carbonate. 

Sodium carbonate (anhydrous). Copper sulphate. 
? ,, (crystals). oxide. 

bicarbonate. turnings, 

hydrogen phosphate. Silver nitrate. 

thiosulphate. Ferrous sulphide. 

,, hydrate,, Piano wire. 

., acetate. Pumice stone. 

sulphite. Indigo. 



INTRODUCTION 



CHEMICALS 

Mercuric chloride. 
Bromine. 
Distilled water. 
Cotton wool. 
Calcium chloride. 

carbonate. 
Iceland spar. 
Barium chloride. 
Platinum chloride. 



REQUIRED (contimted). 

Lead nitrate. 
Pure zinc. 
Litmus. 
Methyl orange. 
Phenolphthalein. 
Alcohol. 
Ether. 
Paraffin. 
Petroleum ether. 



APPARATUS REQUIRED. 



Abel's flash point apparatus. 

Absorption apparatus. 

Accurate balance and weights. 

Agate pestle and mortar. 

Air oven. 

Argand burners. 

Barometer. 

Battery. 

Beakers. 

Bellows. 

Blowpipe. 

Bottles. 

Bunsen burners . 

Burette holders. 

Burettes. 

Calcimeters. 

Calorimeter. 

Clips. 

Clock glasses. 

Condensers. 

Cork borer. 

Corks. 

Crucibles. 



Desiccator. 

Drying tubes. 

Erlenmeyer flasks. 

Evaporating basins. 

File. 

Filter paper (Schleicher and 

Schull). 
Flasks. 
Funnels. 

Gas analysis apparatus. 
Retort stands. 
Glass tubing and rod. 
Graduated flasks. 
Grease pencil. 
Hot plate. 

India-rubber tubing. 
Iron pestle and mortar. 
Measuring tubes. 
Microscope. 
Muffle furnace. 
Nitrometer. 
Phillips beakers 
Pipe-clay triangles 



4 CEMENT CHEMISTS' HANDBOOK 

APPARATUS REQUIRED (continued). 

Pipettes. Spatulas. 
Platinum crucible and capsule. Spotting tile. 

Reagent bottles. Thermometers. 

Retorts. Test-tubes. 

Rough balance. Viscosimeter. 

Rubber bungs. Ware pestle and mortar. 

Sample jars. Wash bottles. 

Sieves. Watch-glasses. 

Specific gravity bottles. Weighing bottles. 

The following works have been consulted in com- 
pilation of this book, and are recommended for 
reference purposes : 

AUTHORS. BOOK. 

Phillips. Engineering Chemistry. 

Stanger and Blount. Reprint from J.S.C.I. on Cement 

Analysis. 

Clowes and Coleman. Quantitative Analysis. 

C. and J. J. Beringer. A Text Book on Assaying. 

Dennis. Hempel's Gas Analysis. 

Kenwood. Public Health Laboratory Work. 

Bayley. Chemist's Pocket Book. 

Meade. (U.S.A.) Portland Cement. 

Eckel. ,, Limes, Plasters, and Cements. 

Taylor. Cement Testing. 

Orton. Hydraulic Cements (Ohio Survey, 

vol. iii.). 



CHAPTER II 
ANALYSIS OF RAW MATERIALS 

Sampling. When sampling a new supply, or 
possible source, of raw materials, great care must 
be taken to obtain an accurate average sample. 

When possible the sampling should be supervised 
by the chemist or other competent person. The 
plan to be followed necessarily varies with the 
situation and material, and must be left to the 
discretion of those on the spot. If possible, samples 
should be taken at different depths as well as in 
different places on the surface of a deposit. Each 
sample should be carefully numbered and labelled 
for reference purposes. Distinct geological layers 
should be specially sampled and separately analysed. 

All the samples should be examined separately, 
and an average sample of the lot should also be 
made and analysed. In the case of large samples of 
fairly dry materials, such as limestone, the material 
should be reduced to a convenient size, thoroughly 
mixed, made into a heap, and sampled by " quarter- 
ing " ; that is, the heap is divided into four equal 
parts diagonally, and an equal amount taken from 
each part ; if necessary, this may be repeated until 



6 CEMENT CHEMISTS' HANDBOOK 

a convenient weight or bulk is obtained. In the 
case of wet clays, etc., greater difficulty will be 
experienced, and these are more readily sampled 
after being allowed to partially dry. If the per- 
centage of moisture in sample is required, however, 
this should be done approximately on as large a 
sample as possible, as well as more accurately in 
smaller quantities as described later. 

(1) Chalk or Limestone. If sufficiently dry, 
break up the sample in a clean iron mortar, and, 
by quartering, obtain a portion for examination 
weighing about 300 grams. Store the remainder 
in a numbered and labelled jar or large bottle for 
reference purposes. Grind the smaller portion by 
hand or in a clean sample mill to all passes through 
the 90-mesh sieve, and place in a clean, dry, stoppered 
bottle for analysis (A). 

(2) Moisture. If very wet and difficult to 
reduce to powder, weigh up on a "decimal" or 
other balance as large a quantity as possible, say 
5000 grams, of the roughly crushed sample. Place 
in a large tin dish or tray and dry over the hot 
plate, taking care that the temperature does not 
rise above 110 to 120 C. When apparently 
quite dry allow to nearly cool, and weigh. 

Loss in weigh t = approximate moisture. 

Repeat if necessary, calculate to percentage. 

As a rule a very approximate estimation of the 
moisture only is necessary. Treat the dry sample 
as in (1). 



ANALYSIS OF RAW MATERIALS 7 

(3) If fairly dry and readily powdered, an accu- 
rate estimation of moisture may be made as follows. 

Weigh out accurately into a flat porcelain weighed 
dish or capsule 5 grams of the sample (A) and place 
in a steam or hot air oven at a temperature of 
100 to 105 C. for one hour. Remove from oven 
and place in a desiccator ; when quite cool weigh 
rapidly ; note weight. Generally one hour's dry- 
ing is sufficient, but the result should be checked 
by replacing in the oven for another twenty minutes, 
cooling and weighing as before. 

Loss in weight x 20 = percentage of moisture 
at 100 C. 

Place the dried materials in a clean, dry, stoppered 
weighing tube, and use for analysis. 

Epitome. 

Break up sample roughly. 
" Quarter " to about 300 grams. 
"Approximate moisture" on hot plate. 
Accurate moisture in oven at 105 C. 
Reserve large sample for reference, dried 
material for analysis. 

(4) Loss on Ignition. Into a weighed platinum 
capsule or crucible weigh out 0*5 gram of the dry 
material and place in a gas muffle at a bright red 
heat for twenty minutes. It is sometimes necessary 
to cover the capsule with a crucible lid during the 
first five minutes of heating to avoid loss by "spurt- 
ing." At the end of the twenty minutes remove 



8 CEMENT CHEMISTS 1 HANDBOOK 

from muffle and allow to cool in a desiccator ; 
weigh. 

Loss in weight x 200 = loss on ignition (or 
C0 2 + H 2 and organic matter). 

Reserve residue for analysis. 

Epitome. 

0'5 gram in muffle for twenty minutes. 
Cool in desiccator and weigh. 

(5) Silica and Insoluble. Brush the ignited 
residue from (4) into a 6- or 7-inch evaporating dish, 
flat form. Cautiously add a.bout 15 c.c. of dis- 
tilled water, rotate to prevent formation of lumps, 
and add 25 c.c. of 10E HC1 ; wash out the platinum 
dish with a little acid into the big dish, and place 
latter on the cooler part of a hot plate or on a water 
bath. 

Evaporate very carefully to dry ness to avoid 
spurting, and then cover with a clock glass and re- 
move to the hottest part of plate and allow to bake 
for one hour. Remove from hot plate, allow to cool 
for five minutes and add 25 c.c. of 10E HC1 and 
warm very gently until the residue is free from 
colour due to iron compounds. Wash down clock 
glass and interior of dish with boiling water from a 
wash bottle. Filter through a 9- or 12-cm. black 
band paper into a 30-oz. Phillips beaker, retaining 
as much as possible of the residue in the dish ; wash 
by decantation thus three times at least, and then 
wash residue into the filter, clean out the dish by 



ANALYSIS OF RAW MATERIALS 9 

means of a rubber-tipped glass rod, and finally with 
the tip of the finger, until every trace of residue is 
contained in the filter paper. 

When filtrate has run through, place the funnel 
and contents, which, as well as all other apparatus 
used, should be distinguished by a number or mark, 
in a drying cone on the hot plate or oven to dry. 
Carefully transfer paper and contents to a weighed 
and marked porcelain crucible, burn off paper over 
a burner or in the mouth of the muffle furnace, then 
ignite in muffle for one hour. Cool in desiccator 
and weigh. 

It is convenient to retain all ppts. obtained during 
analysis for ignition together later. 

Weight weight of crucible = insoluble + filter 
ash. 

Insoluble filter ash x 200 = per cent, silica + 
insoluble. 

Epitome. 

To residue from (4) add 25 c.c. 10E HC1 and 

evaporate to dry ness. 
Take up with 25 c.c. HC1. Filter, wash, weigh. 

Reserve filtrate for (7). 

(6) It is not generally necessary to separately 
estimate the soluble and insoluble Si0 2 , but this 
may be done on another portion of the original 
material as follows. Weigh out 0'5 gram into a 
5 -inch evaporating dish, add water as before, and 
cautiously add 25 c.c. 10E HC1, covering the dish 
as much as possible with a clock glass to prevent 



10 CEMENT CHEMISTS 1 HANDBOOK 

loss. Warm on a hot plate until all soluble matter 
is in solution, then filter this through 9-cm. black 
band paper and wash by decantation, retaining the 
residue in the dish. The filtrate is used for SO 3 
estimation (13). 

Invert the funnel over the dish and wash out any 
trace of residue in the paper. Add 10 c.c. 3E 
Na 2 C0 3 solution and boil for ten to fifteen 
minutes, filter rapidly through the paper previously 
used and wash with boiling water until free from 
alkali or until a drop of filtrate evaporated on a watch- 
glass leaves no residue. Dry, ignite, and weigh. 

Weight ash x 200 = per cent, insoluble residue. 

It may be necessary to estimate H 2 3 in the 
insoluble residue by " fusion." 

Epitome. 

0'5 gram treated with 25 c.c. HC1 warm. 
Filter by decantation, wash. 
Boil residue with 10 c.c. sodium carbonate solu- 
tion. 
Filter, wash, dry, weigh. 

(7) Alumina and Iron Oxide. The filtrate 
from (5) is returned to the dish and warmed until 
nearly boiling upon the hot plate or over an argand 
burner. When nearly boiling add a drop or two of 
bromine water ; continue to warm, but do not boil, 
and add carefully 10E NH 4 OH until a ppt. forms ; 
stir with glass rod and add slight excess. Allow 
to remain on hot plate until nearly free from odour 



ANALYSIS OP RAW MATERIALS 11 

of ammonia, or about fifteen minutes. Filter through 
a 15-cm. black band paper rapidly^and wash with 
boiling water, churning up the ppt. on the filter 
paper with the water jet, until a. drop of the filtrate 
gives no indication of the presence of chloride when 

E 

tested with AgNO 3 solution. Dry and ignite in 

muffle one hour, cool in desiccator, and weigh. 
Weight of ppt. x by200=percent.ofAl 2 O 3 + Fe 2 3 . 

The amount of A1 2 O 3 + Fe 2 O 3 in a limestone is gene- 
rally so small as to render separation unnecessary. 

Epitome. 

Filtrate from (5) ; nearly boil. 

Oxidise with bromine water and ppt. with 

ammonia. 
Warm for fifteen minutes, filter, wash, ignite, 

weigh. 

(8) Lime. The filtrate from (7) is brought 
nearly to boiling-point in a large (40-oz.) Phillips 
beaker. Add a few c.c. of 5E NH 4 OH and boil ; 



whilst boiling, add 50 c.c. of boiling -^- Am. oxalate 

o 

solution, place a watch-glass over beaker and allow 
to steadily boil for five minutes. Remove from the 
direct heat and allow to settle, if possible in a warm 
place, for one hour or longer. 

Filter through a Swedish or white band 15-cm. 
paper into a large bottle or beaker, wash the ppt., 
first by decantation with warm but not boiling 



12 CEMENT CHEMISTS 1 HANDBOOK 

water ; then wash ppt. into the filter paper, removing 
any traces adhering to sides of the beaker by means 
of a rubber-tipped glass rod. 

The lime may be determined volumetrically by 
means of standard permanganate (9) ; or gravimet- 
rically, most conveniently as CaS0 4 (10). The 
filtrate is used for determination of MgO (11). 

(9) Volumetric Determination of CaO. In 

order to avoid accumulation of a bulky filtrate for 
MgO determination, continue washing the calcium 
oxalate ppt. on the paper into another vessel until a 
drop of the filtrate will not discolour a little distilled 
water rendered just pink with a trace of perman- 
ganate solution acidified with 5E H 2 S0 4 . 

Then carefully remove the paper and its contents 
from the funnel, open it out over a large ordinary 
beaker, and wash the ppt. from the paper into the 
beaker ; it is better to complete this operation by 
using a small wash bottle containing 5E H 2 SO 4 . 
Add 15 to 20 c.c. of this acid, make up the contents 
of beaker with water to about 250 c.c., and bring to 
boiling-point. 

Titrate with standard permanganate solution, 
whose strength is known in terms of CaO, until a 
permanent pink colouration is obtained. 

Number of c.c. used x factor x 200 = percentage of 
CaO. 

Per cent. CaO x J 5 <> 6 - = CaC0 3 . 

(lo) Lime as CaSO 4 . Wash calcium oxalate 
ppt. until free from chlorides, dry, place in weighed 



ANALYSIS, OF RAW MATERIALS 13 

platinum crucible with a lid, and ignite gently over 
a bunsen burner to burn off filter paper. 

Remove from burner, allow to cool, and add by 
means of a pipette or glass tube with a fine point, 
drop by drop, pure strong (36E) H. 2 S0 4 , holding the 
lid over the crucible whilst so doing, until the whole 
of the ppt. is moistened with the acid. Heat the 
uncovered crucible over an argand or bunsen burner 
with a rose top, using a very small flame, in a 
draught cupboard until no fumes are evolved. Re- 
place the lid and heat just to redness over a burner 
for about thirty seconds, cool and weigh as CaSO 4 . 

Weight of CaS0 4 x T V ('4117) x 200 = per cent. 
CaO ; or use table (see Appendix 24 A). Calculate 
to CaC0 3 as in (9). 

Epitome. 

(8) Boil filtrate (7) ; add ammonia + 50 cc. 
boiling Am. ox. ; allow to settle, filter, wash. 

(9) Dissolve in 5E H 2 SO 4 + H 2 O, boil, titrate 
with standard potassium permanganate. 

(10) Dry, ignite, add sulphuric acid in platinum 
crucible, drive off sulphuric acid, weigh as 
CaS0 4 . 

(n) Magnesia. Evaporate the filtrate from (8) 
nearly to dr} r ness in the large dish ; add 30 c.c. 16E 
HNO 3 and heat on hot plate in draught cupboard 
until no more ammoniacal salts are volatilised. 

Remove from plate, allow to cool ; then add about 
5 c.c. of 10E HC1 and about 20 c.c. of water. Warm 
and add slight excess of 10E NH 4 OH ; filter off 



14 CEMENT CHEMISTS' HANDBOOK 

the small ppt. of Si0 2 ,Al 2 3 ,Fe 2 3 through a 5-cm. 
black band paper and wash. This may generally be 
ignored as being due to impurities in the reagents 
and from the vessels used. 

To the filtrate, which should not exceed 100 c.c. 
or so, when cool add at least 10 c.c. of 20E NH 4 OH, 

9TT 

then 5 c.c. of -Q- Na 2 HPO 4 solution. Stir well with 

a rubber- tipped rod, but avoid touching the sides of 
the beaker as much as possible, and place in a dish 
of water or other cool place to settle for twelve hours 
(over night) if time permits. 

When the ppt. has completely settled, filter 
through a 7- or 9-cm. Swedish or white band filter 
paper, wash by decantation, using 5E NH 4 OH ; then 
transfer ppt. to the paper, rub out carefully any 
particles adhering to side of beaker, and wash on the 
paper until a drop of the filtrate, when acidified with 

Tfi 

nitric acid gives no ppt. with -^ AgNO 3 solution. 

It is important that the washing should be com- 
plete, but not excessive. 

Ignite, best in a platinum crucible, first at a low 
temperature over a bunsen burner and then at a 
higher temperature ; or in a muffle furnace for twenty 
minutes. Cool in a desiccator and weigh as Mg 2 P 2 O 7 . 

Weight of Mg 2 P 2 O 7 x T 4 r T or ('3619) x 200 = per 
cent. MgO ; or use table (Appendix 25 A). 

Per cent. MgO x f == per cent. MgC0 3 . 



ANALYSIS OF RAW MATERIALS 15 

Epitome. 

Evaporate lime filtrate to dry ness. 

Add 30 c.c. 16E HN0 3 and drive off ammonium 

compounds. 
Take up with 5 cc. hydrochloric acid, ppt. with 

10E NH 4 OH. 
Filter, wash, cool. Add 20 c.c. 10E NH 4 OH 

and 5 cc. sodium phosphate solution, stir. 
Allow to settle, filter, wash with 5E NH 4 OH. 
Dry, ignite, weigh as Mg 2 P 2 7 . 
Calculate to MgO or MgC0 3 . 

(12) Alkalies are generally estimated by differ- 
ence, but the method described under Clay (31) or 
Cement (122) may be adopted if necessary. 

(13) Sulphates. Boil the filtrate from (6) and, 
whilst still boiling, add 10 c.c. of E BaCl 2 solution ; 
after five minutes allow to settle in a warm place 
for a few hours. Filter through a 7-cm. No. 417A 
Max DreverhofFs paper, wash with warm water 
until free from chloride, dry, ignite, and weigh as 
BaS0 4 . 

Weight of BaS0 4 x -gfo x 200 = per cent, of 
S0 3 (see Appendix 26 A). 

Epitome. 

Filtrate from (6). Boil, add 10 c.c. E BaCl 2 . 
Allow to settle, filter, wash, ignite, weigh as 
BaS0 4 . 



16 CEMENT CHEMISTS' HANDBOOK 

(14) Accurate Estimation of Carbon Di- 
oxide. One gram of the limestone is decomposed by 
hydrochloric acid in a flask, the carbon dioxide 
evolved is absorbed by potassium hydrate solution, 
after passing over various reagents, and weighed. 

The following apparatus must be fitted up. The 
lettering refers to the illustration. (Fig 1.) 

A fairly wide-mouthed flask (A) is fitted with a 
three-holed rubber bung ; through one hole is passed 
a stoppered funnel (b) ; a tube (a), containing soda- 
lime, is passed through one of the other holes ; and 
the remaining one is fitted with a glass tube which 
is connected to the absorption apparatus. A two- 
holed bung may be used, in which case the funnel 
is substituted by a pipette connected at the upper 
end with the soda-lime tube, a Mohr's clip being 
placed on the connecting rubber, and this is released 
when the acid has to enter the flask. The tube 
leading from the flask is connected by rubber, first 
with bulbs (.Z?) containing strong sulphuric acid ; 
secondly, to a U-tube ((7), the nearer limb of which 
is filled with copper sulphate pumice, and the other 
limb with solid calcium chloride. Connected to 
this tube are the potash bulbs (D), in which the 
GO 2 has to be absorbed and weighed ; arid these 
are in turn connected to a straight calcium chloride 
tube, which is also weighed with the bulbs. 

The absorption bulbs should be filled with 5E KOH 
solution in sufficient quantity to fill the lower half 
of the bulbs and to be contained in the large pear- 
shaped bulb should there be any back pressure. 



ANALYSIS OF RAW MATERIALS 



17 



The whole apparatus is connected with an aspirator 
made from a Winchester quart bottle as shown. 




Instead of potash bulbs, a U-tube containing 
soda-lime may be used. 



18 CEMENT CHEMISTS' HANDBOOK 

Stoppered U -tubes are to be preferred to corked 
ones ; if the latter are used, they should be made 
air-tight with paraffin \vax. 

A little cotton-wool should be placed before and 
after the CaCJ 2 and pumice-stone in the tubes, to 
prevent the passage of fine dust. 

All rubber connections should be wired on and 
the apparatus tested before use. When the appa- 
ratus is ready for use, detach the absorption bulbs 
or tube arid the CaCl 2 straight tube ; stop up the 
open end of the rubber tube by means of a bit of 
glass rod. See that the bulbs and tube are quite 
dry, and weigh. 

Weigh out into the flask 1 gram of the material, 
cover it with water. Place 50 c.c. of 5E HC1 in the 
funnel or pipette, and reconnect up the whole appa- 
ratus, except the aspirator. Close the air inlet 
through the soda-lime tube. 

Allow acid to drop slowly on the carbonate so 
that the bubbles of air driven from the apparatus 
may be easily counted as they pass through the 
sulphuric acid ; continue addition of the acid until 
effervescence ceases. 

Close the stopper of the funnel, or, if a pipette, 
carefully push the point under the surface of the 
liquid, attach the aspirator and set it in action. 
Place an argand burner under the flask and warm 
gently. Open the air inlet tube so that a current 
of air is made to pass through the apparatus until 
quite half the water in the aspirator has run out. 
Then stop the operation, disconnect and stopper up 




ANALYSIS OF RAW MATERIALS 19 

the weighed bulbs, allow to get quite cool, and 
weigh. 

Increase in weight x 100 = per cent. CO 2 . 

Epitome. 

One gram decomposed by hydrochloric acid in 

the absorption apparatus. 
C0 2 absorbed in potash or soda-lime, and 

weighed. 

(15) Rapid Estimation of CO 2 . A rapid and 




Yi&. 2. APPABATUS FOE RAPID ESTIMATION OF C0. 2 . 

fairly accurate estimation of carbon dioxide may be 
made in the apparatus represented in Fig. 2. 

Fit a wide-mouthed 4-oz. flask with a rubber 
bung. Through one hole place a piece of glass 
tube attached to a straight Cad 2 tube. Through 



20 CEMENT CHEMISTS 1 HANDBOOK 

the other hole run a piece of glass tubing closed at 
the outer end with a small piece of rubber tubing 
and glass rod. 

A small piece of cotton-wool is first placed in the 
bulb tube, and the bulb is then filled with dehy- 
drated copper sulphate pumice followed by granular 
CaCl 2 in the straight part ; another piece of wool 
is then inserted and the tube closed with a cork 
bearing a small glass tube. 

Thoroughly dry the apparatus, weigh out 1 gram 
of the carbonate and brush it into the flask ; cover 
with water, and then lower a small glass or gutta- 
percha test-tube containing about 7 c.c. of 5E HC1 
into the flask by means of a piece of cotton. Insert 
the stopper so that the cotton from which the test 
tube is suspended is held in place. 

Weigh the whole apparatus and contents. Slightly 
tip the apparatus so that the acid is caused to leave 
the test-tube a little at a time. When effervescence 
has ceased, warm the flask over an argand burner 
for about five minutes ; allow it to cool somewhat, 
and then draw, by means of an aspirator as in (14) 
or by the mouth, a current of air through the appa- 
ratus, for this purpose removing the rubber cap of 
the inlet tube. Allow the apparatus to cool, see 
that the exterior is quite dry, and weigh complete 
as before. 

Loss in weight x 100 = per cent. C0 2 . 

A determination can be made in about thirty 
minutes. 



ANALYSIS OF RAW MATERIALS 21 

Epitome. 

Weigh into prepared flask 1 gram. 
Decompose with hydrochloric acid, warm, cool, 
weigh. 

The total carbonate in an ordinary chalk or lime- 
stone may be rapidly estimated as CaCO 3 upon one 
of the calcimeters described in chapter iii., and 
especially conveniently upon Slater's instrument, 
using the Tables given in Appendix (27 A" and 28A). 

A dolomite or magnesian limestone is insoluble 
in cold hydrochloric acid, and therefore the C0 2 
cannot be estimated upon a calcimeter. Of course, 
for Portland cement manufacture to standard speci- 
fications such limestones are useless, and therefore 
of no importance. 

Should an analysis of such material be required, 
the methods previously described (5, 6, 7, 8) may 
be used ; but care must be taken that throughout 
the analysis there is a sufficient quantity of ammo- 
nium chloride present to prevent the precipitation 
of magnesium as Mg(OH) 2 by ammonia. 

In reporting the result of an analysis of a chalk 
or limestone, it is generally sufficient to state total 
lime as CaO, and its equivalent of CaC0 3 separately, 
MgO, loss on ignition (which includes CO 2 , H 2 O, and 
organic matter), silica, ferric oxide and alumina ; and 
alkalies by difference. 



$2 CEMENT CHEMISTS' HANDBOOK 

MARLS, GAUL/T CLAY, CALCAREOUS 
SHALES. These materials, as found in the 
British Isles, are intermediate in chemical com- 
position between limestones and true clays and 
shales. 

The method adopted for analysis must largely 
depend upon the particular material under exami- 
nation ; when the calcium carbonate is present in 
the proportion of 70 to 75 per cent., the processes 
described under Limestone (1 and following) may be 
used. When the CaC0 3 does not exceed 25 per 
cent., the methods to be described for clays and 
shales may be used, care being taken that, after 
treatment with sulphuric acid, sufficient 10E HC1 
is used to take up all the CaS0 4 formed, or this will 
be included erroneously in the " insoluble." 

The following method giving total Si0 2 , Fe 2 O 3 , 
A1 2 3 , GaO, and MgO may be used in most cases 
satisfactorily. 

(16) Weigh into a capacious p ] atinum crucible or 
capsule '5 gram of the dry sample (3), and ignite in 
muffle at a good red heat for twenty minutes. Cool 
in desiccator and weigh rapidly. 

Loss in weight x 200 = percentage loss on 
ignition. 

(17) Mix the ignited residue with about 5 grams 
of fusion mixture (K 2 C0 3 ,Na 2 CO 3 ) in the platinum 
crucible or large capsule, using the smooth end of a 
glass rod to incorporate the contents. 

Heat carefully over a bunsen burner for about 



ANALYSIS OF RAW MATERIALS 25 

ten minutes, and then over a blast burner or in a 
muffle until the mixture is in a state of quiet, com- 
plete fusion. Rotate the crucible to spread the 
fused mass as much as possible, and then allow to 
cool rapidly by standing in a little cold water or on 
a cold slab. Place in a large evaporating basin, 
cover with distilled water and digest on hot plate 
until the mass has broken up and the crucible and 
lid can be washed clean. If necessary, a little 5E 
HC1 may be used to ensure the crucible being clean. 
Then add sufficient 10E HC1, a little at a time, 
covering the dish as far as possible with a clock 
glass to prevent loss, until a clear solution is 
obtained. 

Evaporate slowly on the hot plate or air bath 
almost to dryness, remove and add about 10 c.c. of 
10E HC1, and wash any material from the clock 
glass and sides down into the bottom of dish. 
Evaporate slowly to dryness, if necessary breaking 
up any lumps that form with the end of a glass 
rod ; when dry, bake on the hot plate for at least 
one hour. 

Remove from the hot plate and, when nearly 
cool, add 25 c.c. 10E HC1 and sufficient water to 
dissolve the chlorides formed. 

Filter through a 12^-cm. black band paper and 
wash well. After fusion, all the washings require 
to be very thorough. Repeat the evaporation and 
filter off any trace of Si0 2 , and add to that first 
obtained. 

Dry, ignite, and weigh. 



24 CEMENT CHEMISTS 1 HANDBOOK 

Weight - filter ash x 200 = per cent. SiO 2 . 

Estimate Al 2 O 3 + Fe 2 3 , as in (7); but if Fe 2 O 3 
is required separately, take 1 gram of substance 
for analysis and follow the plan described under 
Clay (24), making the solution up to a known 
volume, and divide into two portions, using one 
portion for volumetric determination of Fe 2 3 (25, 
26, 27). 

Estimate CaO as in (8) and MgO as in (11). 

Epitome. 

Fuse '5 or 1 gram with fusion mixture. 
Dissolve mass in water and hydrochloric acid. 
Evaporate to dryness, bake, cool, take up with 

water and hydrochloric acid. 
Filter, wash, and weigh Si0 2 . 
Ppt. A1 2 3 , Fe 2 3 with ammonium hydrate (7). 
Filter, wash, weigh. 
Ppt. CaO with ammonium oxalate (8). 
Filter, wash, estimate. 

Evaporate to dryness, add 30 c.c. nitric acid. 
Estimate MgO as Mg 2 P 2 7 (11). 

(18) CLAY. A mechanical analysis of clay, 
except for brickmaking, is not often required. 
When necessary it must be carried out on the 
undried samples by elutriation. For this purpose 
an apparatus specially made may be used, or a 
series of bottles or iars can be fitted up as 
follows. 



ANALYSIS OF RAW MATERIALS 25 

Choose three wide-mouthed bottles and fit them 
with sound corks, each bored with two holes to 
carry fairly large glass tubing, in each case one 
piece being carried to the bottom of the vessel and 
the other just through the cork. The longer tube 
of the first bottle is connected to a water tap, the 
smaller piece to the succeeding bottle, and so on, so 
that a stream of water may be run through the 
whole apparatus, the overflow from the last bottle 
being caught in a large jar or pail. 

A weighed amount, say 100 grams, of the clay is 
placed in the bottle attached to the tap and a gentle 
stream caused to circulate through the apparatus 
until the overflow water comes over quite clean. 
The water is then turned off, and the material in 
the bottles allowed to subside. The bulk of the 
water is poured away, and the solid matter washed 
out into a weighed dish, dried, and weighed. The 
residues being reported as coarse (sand), medium, 
fine, and very fine by difference. If necessary, the 
fineness of each portion upon standard sieves may 
be taken. As stated previously, however, upon a 
cement works using modern machinery the physical 
condition of the raw material is of little importance 
compared with the chemical composition. 

The moisture should be " approximately esti- 
mated " (2), and the whole sample, when dry, 
powdered. A smaller sample obtained by quarter- 
ing should then be dried in the air oven and 
kept for analysis in a weighing tube or stoppered 
bottle. 



26 CEMENT CHEMISTS' HANDBOOK 

(19) Estimation of Si0 2 (sand), A1 2 3 , Fe 2 O 3 , 
CaO, and MgO. Weigh into a large porcelain or 
platinum dish 1 gram of the dry powdered clay 
and cover with 20 c.c. 36E H 2 S0 4 ; rotate cautiously 
to break up any lumps, cover with a clock glass, 
and heat very gently best over an argand burner 
for 10 hours (over night). In the morning remove 
the clock glass and increase the heat sufficiently to 
steadily drive off the sulphuric acid. 

When no more fumes are driven off, place on 
the hot plate for about twenty minutes. Remove 
from the hot plate, allow to cool somewhat, and 
then add 25 c.c. of 10E HC1 and a little distilled 
water. 

Filter through a 12 '5 -cm. black band paper, 
retaining the insoluble matter in the dish. Add 
another 25 c.c. of hydrochloric acid, digest on the 
hot plate for a few minutes, add water, and filter 
as before. 

Repeat this operation, using altogether 75 c.c. of 
acid, then wash by decantation until free from 
chlorides, and when cold make filtrate up to 500 
c.c. (24). 

Wash any material upon the filter paper back 
into the dish and boil with 25 c.c. of 5E Na 2 CO 3 
solution or with 1 gram of sodium carbonate 
crystals and sufficient water, for about fifteen 
minutes. Filter, whilst still hot, through a 12'5- 
cm. black band paper, and wash with boiling water 
until quite free from any trace of alkali. Reserve 
filtrate for SiO 2 estimation (23). 



ANALYSIS OF RAW MATERIALS 27 

Dry residue, ignite in platinum crucible, and 
weigh. 

Weight ash x 100 = per cent, insoluble, sand, &c. 

(20) After weighing, treat the insoluble matter 
in the platinum crucible with about 5 c.c. of hydro- 
fluoric acid and a few drops of 36E H 2 S0 4 , warm 
over a small argand flame in a good draught cupboard 
until no further fumes are evolved. Repeat three 
times, when there should be only a small residue 
remaining. 

Treat this residue with 10E HC1, warm in a 
small dish or beaker, and filter through a 7-cm. 
paper, wash, dry, ignite, and weigh as TiO 2 . 

Weight- ash x 100 = per cent. TiO 2 . 

(21) In the filtrate from above, estimate (7) 
A1 2 3 , Fe 2 3 (R 2 3 ). 

Weight ash x 100 = per cent. R 2 O 3 in insoluble. 

It is usual then to calculate the R 2 O 3 to felspar 
6SiO 2 .Al 2 O 3 .Na 2 O thus : 

Per cent. R 2 O 3 x 3*5 = per cent. SiO 2 . 

Per cent. R 2 O 3 x *6 = per cent. Na 2 O. 

Per cent, insoluble -(Si0 2 + R 2 O 3 + Na 2 O + TiO 2 ) 
= per cent, quartz. (See Appendix for example.) 

The insoluble matter can then be reported as shown 
in Appendix [1A]. The result thus obtained is not 
absolutely accurate, but suffices for most purposes. 

(22) Instead of treating the residue (19) with 
hydrofluoric acid, the SiO 2 and A1 2 O 3 can be esti- 
mated by fusion as in (17). 



28 CEMENT CHEMISTS' HANDBOOK 

(23) Acidify with 10E HC1 the alkaline filtrate 
from the insoluble estimation (19), and evaporate 
carefully to dryness in a platinum or porcelain dish ; 
bake for half an hour, allow to cool, and then take 
up with water and a little 10E HC1, filter through 
a 12 "5 -cm. paper and wash till free from chloride. 
Dry, ignite in muffle for one hour, and weigh. 

Weight filter ash x 100 = per cent. Si0 2 . 

(24) The filtrate, which has been made up to 500 
c.c., is divided into equal portions of 250 c.c. In one 
part the A1 2 3 , Fe 2 3 , CaO, and MgO are esti- 
mated as in (7) (8) and (1 1). If small in amount the 
calcium oxalate ppt. may be converted into CaO over 
a blast burner or in the muffle and weighed as such. 

(25) Estimation of Fe 2 3 . The A1 2 3 , Fe 2 3 
is pptd. as in (7), filtered and washed slightly ; it 
is then redissolved in dilute acid and the iron 
estimated volumetrically after reduction, using 
standard potassium permanganate or bichromate 
solution. 

(26) Estimation of Iron by means of 
Standard Permanganate. Dissolve the ppt. of 
A1 2 3 , Fe 2 O 3 in 5E H 2 S0 4 and wash into an 
Erlenmeyer flask, add fair excess of the acid and a 
few small pieces of pure zinc. Fit the flask with a 
cork bearing a bunsen valve, i.e., a piece of glass 
tube to which is attached a piece of rubber tubing 
having a longitudinal slit and closed with a glass 
rod or clip, and place in a slightly warm place until 
reduction is complete. This is approximately indi- 



ANALYSIS OF RAW MATERIALS 29 

cated by the solution becoming colourless, when a 
drop should be withdrawn on the end of a glass 
rod and tested by means of ammonium or potas- 
sium sulphocyanide solution, the reduction being 
complete when there is no pink colouration with 
that reagent. 

Filter the reduced iron solution rapidly and wash 
into a clean flask ; if necessary, add more sul- 
phuric acid ; and titrate with standard permanganate 
[17 A] solution until a permanent pink colour is 
obtained. 

No. of c.c. x Fe 2 3 factor x 200 = per cent. Fe 2 3 . 

Subtract from A1 2 O 3 , Fe 2 3 found (24) = A1 2 O 3 . 

(27) Estimation of Iron by means of 
Standard Bichromate. Dissolve the ppt. of 
A1 2 3 , Fe 2 O 3 in 5E HC1, as small a quantity as 
possible, wash into an Erlenmeyer flask fitted with 
bunsen valve, dilute to about 200 c.c., and add 20 
c.c. of 2E Na 2 SO 3 . Boil for twenty minutes or 
until free from S0 2 . Cool as quickly as possible 
and test as above ; if reduction is complete, titrate 
with the standard bichromate [ISA]. On a clean 
spotting tile have ready a number of drops of freshly 
prepared, very dilute potassium ferricyanide solu- 
tion, run the bichromate solution, at first a few c.c, 
at a time, later drop by drop, into the iron solution ; 
after every addition abstract a drop by means of a 
glass rod and place in contact with the "spots" of 
ferricyanide. The reaction is complete when no 
blue or green tint is produced with the ferricyanide. 

No. of c.c. x Fe 2 3 factor x 200 = per cent. Fe 2 O 3 . 



30 CEMENT CHEMISTS 1 HANDBOOK 

Epitome. 

Treat 1 grain for ten hours with 36E H 2 S0 4 , 

dry and bake. 
Take up with three portions 10E HC1, filter, 

wash. 

Residue = SiO 2 and insoluble. 
Boil residue with 25 c.c. 3E Na 2 CO 3 . 
Filter, wash, residue = insoluble. 
Filtrate, acidify, evaporate = SiO 2 . 
Filtrate from insoluble = A1 2 O 3 , Fe 2 O 3 , CaO, 

MgO(7, 8, 11,25). 

(28) Loss on Ignition. Ignite '5 grarn of the 
powdered and dry sample for twenty minutes in a 
muffle. Cool in desiccator and weigh rapidly. 

Loss in weight x 200 = per cent, loss on ignition. 

If an ultimate analysis only is required this 
residue (28) may be treated as (17) and the 
11 rational " method (19) omitted. 

(29) Total Sulphur. One gram of the dry 
sample is mixed with 10 grams of a finely powdered 
mixture of Na 2 CO 3 (10 parts) and KNO 3 (1 part) 
and heated to quiet fusion in a covered platinum 
crucible. 

The fused mass is dissolved in water, acidified 
with 10E HC1, and filtered, if necessary. The 
filtrate is boiled and to it, whilst still gently boiling, 
is added 10 c.c. of E BaCl 2 ; after a few minutes the 
ppt. is allowed to settle in a warm place for some 



ANALYSIS OF RAW MATERIALS 31 

hours, filtered through an S0 3 paper, washed, dried, 
and ignited and weighed as BaS0 4 . 

Weight of BaS0 4 x *137 x 100 = per cent, sulphur. 

This may be calculated to iron pyrites FeS 2 . 

Epitome. 
Fuse with sodium carbonate and potassium 

nitrate. 

Take up with hydrochloric acid, filter, wash. 
Ppt. with barium chloride solution, weigh as 

BaS0 4 . 

(30) Sulphur present as Sulphate. Weigh 
out 1 gram of the sample into an evaporating dish, 
add a little water and 25 c.c. of 10E HC1, warm 
twenty to thirty minutes, then add 10 cc. of 10E 
HC1 and water. Filter and wash. Treat the 
filtrate as in (29). 

Weight of BaSO 4 x -343 x 100 = per cent. S0 3 . 

If this is calculated to CaSO 4 its equivalent of 
CaO must be deducted from the amount found. 

Thus per cent. SO 3 x 17 = per cent. CaS0 4 . 
For each TO per cent. CaSO 4 deduct '41 per 
cent, from CaO. 

The sulphur present as sulphate must be deducted 
from total sulphur found, in order to obtain sulphur 
present as sulphide. 

(31) Alkalies. Soda and potash may conven- 
iently be estimated as follows this method being 
known as Laurence Smith's : 



32 CEMENT CHEMISTS 1 HANDBOOK 

Mix in an agate mortar 1 gram of the dry clay 
with its own weight of pure ammonium chloride and 
6 grams of pure precipitated chalk ; should there be 
any calcium carbonate present in the clay, this must 
be allowed for. Place the mixture in a platinum 
crucible and heat gently at first over a buiisen burner 
and then for one hour at a red heat, keeping the 
crucible covered ; cool, turn the mass out into an 
evaporating dish, and wash out the crucible with 
distilled water into the dish. Dilute somewhat, heat 
to boiling, filter, and wash into a beaker. Add 1*5 
grams of solid ammonium carbonate, evaporate to 
about 50 c.c., add a little more carbonate + 
ammonia ; then filter and wash. Evaporate the 
filtrate to dryness in a weighed platinum dish, heat 
gently at first to drive off ammonium chloride and 
then to a dull redness ; cool in desiccator and weigh. 

The weight = KC1 + NaCl. 

(3ia) Separation of Soda and Potash. 

Dissolve the mixed chlorides in about 5 c.c. of water 
and add sufficient E PtCl 4 to convert into the double 
chlorides, assuming the whole to be NaCl, 117 grams 
of which require 336*38 grains of PtCl 4 . One c.c. of 
E PtCl 4 solution contains '0841 gram. The mixture 
is then taken nearly to dryness on the water bath and 
15 c.c. of alcohol added ; the dish is then allowed to 
stand for three hours with an occasional rotation. 

When the ppt. has well settled, the clear liquid is 
poured off through a filter paper which has been 
dried and weighed, the ppt. is washed by decantation 



ANALYSIS OF RAW MATERIALS 33 

with alcohol and thus transferred to the filter paper 
and again washed, using a small wash bottle con- 
taining alcohol until filtrate is colourless. The paper 
and K 2 PtCl 6 are then dried in an air or steam oven 
at 100 C., cooled in a desiccator, and weighed. 

Weight -weight of filter paper x -3070 = KC1. 
Subtract this from weight of mixed chlorides = 

NaCl. 

KC1 x -63204 x 100 = per cent. K 2 O. 
NaCl x -53077 x 100 = per cent. Na 2 0. 

Epitome. 

(31) Fuse with ammonium chloride and calcium 

carbonate. 

Digest with water, filter, and wash. 
Add ammonium carbonate, filter, and wash. 
Evaporate to dryness. 
Ignite, weigh. 

(3ia) Dissolve in water, ppt. with PtCl 4 and 

alcohol, filter. 
Wash with alcohol, weigh on tared paper. 

For cement-making purposes an accurate deter- 
mination of K 2 and Na 2 O is not often necessary, 
but an estimation of the soluble chloride (NaCl) is 
sometimes useful. 

(32) Soluble Chloride. Treat 5 grams, or 
more if necessary, with distilled water in a flask or 
beaker, and warm. Filter and wash well. Estimate 
the chloride in the filtrate by means of standard 



34 CEMENT CHEMISTS 1 HANDBOOK 

N 

7. AgN0 3 , using potassium chromate solution as 

indicator, as described under Water. 

No. of c.c. x -00585 x 20 = per cent. Nad. 

Shales, Sandstones, and Slates. The methods 
adopted for the analysis of these materials must 
depend upon individual circumstances. As a rule 
the following processes, already fully described, will 
be found suitable : 

Moisture (3), loss on ignition (4), followed by 
fusion (17) and estimation of the Si0 2 (17), 
A1 2 3 Fe 2 3 (7), CaO (8) and MgO (11). 

Natural Cement Rock. This may generally 
be treated as a limestone, carrying out the following 
estimations : 

Loss on ignition (4), silica and insoluble (5 and 6) 
or a fusion of the insoluble may be made 
(17), A1 2 3 Fe 2 3 (17), CaO (8 and 9), 
magnesia (11), C0 2 (14 or 15) if necessary or 
CaC0 3 and MgC0 3 may be obtained by cal- 
culation ; sulphates (13) and sulphides (29). 

(33) Slags. Weigh out '5 gram of the finely 
powdered sample into a platinum crucible and fuse 
with 3 grams of fusion mixture ; separate the 
SiO 2 , as in (17); but for accurate work it is 
necessary to evaporate to dryness after filtering to 
separate the remaining traces of Si0 2 . 

(34) The filtrate from the silica is warmed in a 
capacious beaker; a little solid and then 5E 
Am 2 C0 3 solution added until a ppt. just forms. 



ANALYSIS OF RAW MATERIALS 35 

Then add a drop or two of 5E Acetic acid and 
excess of 4E Sodium acetate solution. Boil gently 
for ten minutes and filter, whilst still hot, through 
a 15-cm. black band paper; wash. 

The filtrate must be clear and colourless and is 
used for manganese estimation (36). 

(35) Kedissolve the pptd. basic acetates of iron 
and alumina in 10E HC1 and ppt. with ammonia, 
wash, dry, ignite, and weigh as A1 2 3 , Fe 2 O 3 and 
P 2 O 5 if present (7). 

(36) Add the second filtrate to that obtained from 
the acetate separation (34) and concentrate some- 
what, cool and then add 3 c.c. of bromine, and stir 
until it has gone into solution, add 20 c.c. of 
20E NH 4 OH and boil for twenty minutes, filter, 
wash, ignite, and weigh as Mn 3 O 4 . 

Weihgt-ash x 7205 x 200 = per cent. Mn. 
Or, calculate to MnO 2 or MnO. 

Epitome. 

Separate iron and alumina as basic acetates. 
Add bromine and ammonia, filter, wash. 
Weigh as Mn 3 O 4 . 

(37) In the filtrate estimate CaO (8) and MgO 

(a). 

(38) The iron present should be estimated in 
another portion of 1 gram by fusion, as in (33) ; the 
iron should be separated as basic acetate, redissolved 
in hydrochloric acid, reduced as in (27), estimated 



36 CEMENT CHEMISTS 1 HANDBOOK 

by standard bichromate, and calculated to ferrous 
oxide. 

No. of c.c. x FeO factor x 100 = per cent. FeO. 

This must also be calculated toFe 2 O 3 ,and subtracted 
from the weight of A1 2 3 and Fe 2 O 3 and P 2 5 found 
(35), in order to obtain A1 2 3 and P 2 5 if present. 

Should the iron present both as ferric and ferrous 
oxide be required, the process and apparatus recom- 
mended by Averyand described in Phillips' B Engineer- 
ing Chemistry, p. 108, maybe followed. 

An alternative method is to make the filtrate from 
Si0 2 (33) up bo a known bulk and then take half that 
quantity for estimation of A1 2 3 , Fe 2 3 , CaO, and 
MgO, and use the other portion for estimation of 
iron. 

(39) Phosphorus and Sulphur. Fuse 2 grams 
at least of the sample with sodium carbonate and 
potassium nitrate, treat the melt with hot water 
until it disintegrates, boil, filter off the bases, and 
wash well. Allow the filtrate to cool and make up 
to 500 c.c. Divide into two portions (A) and (B). 
Acidify A with HN0 3 and add a large excess of 
ammonium molybdate solution, allow to stand for 
twelve hours, at about 50 C. ; if the temperature 
is allowed to rise, any arsenic present will also be 
pptd. Pour off the clear liquid through an S0 3 
paper, and test with a little more molybdate 
solution to ascertain whether all phosphate has 
been pptd. ; if so, filter and wash any ppt. adhering 
to beaker with E HN0 3 . Then, using a fresh 
beaker to collect the filtrate, dissolve the ppt. in 



ANALYSIS OF RAW MATERIALS 37 

5E NH 4 OH, rinse out the beaker, and wash the 
filter paper well. 

Add excess of magnesia mixture, treat as in (11). 
Weight of Mg 2 P 2 O 7 x -638 x 100 = per cent. 

PA. 

Epitome. 

Fuse with sodium carbonate and potassium 
nitrate. 

Dissolve in water, acidify with nitric acid, 
ppt. with ammonium molybdate, dissolve in 
ammonia, ppt. with magnesia mixture. 

Subtract from A1 2 O 3 + P 2 5 and Fe 2 O 3 (35). 

(40) Sulphur. Acidify (B) with 10E HOI, add 
10 c.c. E BaCl 2 solution, treat as in (29). 
BaS0 4 x -137 x 100 = per cent, sulphur. 



CHAPTER III 

CALCULATION OF PROPORTION 
OF RAW MATERIALS 

FROM the analysis of any given material it is 
possible to estimate its usefulness for cement 
making within certain limits. With entirely untried 
materials actual tests on as large a scale as possible 
should be carried out. 

Any of the larger English and American text- 
books on cement manufacture contain full informa- 
tion as to the ideal composition. 

LIMESTONES. Unless a calcareous clay or 
shale is to be used, the CaCO 3 content must reach 
75 per cent. A poor limestone may sometimes be 
enriched by using a purer stone to raise the per- 
centage of CaC0 3 . About 2 per cent. MgO renders 
the stone useless for cement making to standard 
specification ; it is desirable that only 1 per cent, or 
less be present. 

For use with rotary kilns, a little sulphur as 
sulphide or sulphate is immaterial either in the 
stone or clay. 

38 



PROPORTION OF RAW MATERIALS 39 

CLAY, SHALES, Etc. The proportion of 
SiO 2 to A1 2 O 3 + Fe 2 3 should be 2 J or 3 to 1. That 
is, per cent. SiO 2 should equal per cent. R 2 O 3 x 3, 
unless working with a siliceous limestone or a stone 
of nearly correct proportions which is only deficient 
in one constituent. 

A high percentage of Fe 2 3 is, for ordinary 
purposes, undesirable. Very siliceous materials 
produce a slow-setting cement and the mixture 
requires burning at a high temperature. Highly 
aluminous materials produce an easily burnt clinker, 
but the cement is generally very quick-setting and 
otherwise unsatisfactory. 

A clay containing nodules of iron pyrites should 
be avoided, as a source of possible, if not probable, 
trouble. 

Calculation from Formulas. Several for- 
mulas exist whereby the proportions may be cal- 
culated in which raw materials should be mixed, 
but even the best of these only serve as a rough 
guide in actual practice. From experience 
the most favourable data to work upon is 
the percentage of CaCO 3 , as this can be 
readily checked and altered. The percentage of 
CaC0 3 in a raw mixture never varies greatly from 
75 per cent. 

In order to obtain approximately the correct pro- 
portions, proceed as follows. For example, see 
Appendix [3 A]. 

(1) From per cent. CaCO 3 in limestone deduct 75 




40 CEMENT CHEMISTS' HANDBOOK 

or per cent, required in mixture ; the result should 
be the weight of clay or shale required. 

(2) From 75 or per cent. CaC0 3 required in 
mixture deduct per cent. CaC0 3 in clay or 
shale ; the result should be weight of limestone 
required. 

Of course, the weights so obtained can be read 
as grams, lb., cwts., tons, or any unit required. In 
each case, when using raw damp material, the 
moisture must be estimated and allowed for, as 
obviously more will be required than when using 
perfectly dry stone or clay. 

As a result of researches into the composition of 
an ideal Portland cement, various experimenters 
have put forward formulas for preparing the raw 
mixture when the composition of the materials is 
known. The following will be found a good working 
formula : 

(1) Multiply per cent. Si0 2 in limestone by 2*8 ; 
multiply per cent. A1 2 3 in limestone by I'l, and 
add the products. 

(2) Deduct result from per cent. CaO in stone = 
per cent. CaO available for combination with 
clay (y). 

(3) Per cent. Si0 2 in clay x 2'8 + A1 2 3 in clay x 
1-1, gives CaO required by 100 parts of clay. 

Deduct per cent. CaO in clay and remainder = 
amount required to be added (x). 

As the available CaO (2) in 100 parts of limestone 
is known, by simple proportion, parts of limestone 
to be added can easily be calculated. Thus let x = 






PROPORTION OF RAW MATERIALS 41 

amount of CaO required for 100 parts of clay, and 
y = per cent, available in limestone ; 

then - - = parts of stone to each 100 parts of clay. 
For examples worked out, see Appendix [2A]. 



ANALYSIS OF SLURRY AND OTHER 
RAW MIXTURES 

SLURRY. In order to obtain an average 
sample of the slurry being washed, the constant 
supervision of the chemist or of a trustworthy 
assistant is absolutely essential. Owing to different 
prevailing conditions, it is impossible to lay down 
any fixed plan of sampling. As a rule, samples 
should be taken at regular short intervals as the 
slurry leaves the grinding plant ; these should, at 
longer intervals, be thoroughly mixed and a smaller 
average sample taken for examination. 

For sampling slurry-mixing tanks or silos various 
devices exist, the simplest, perhaps, being a tin can 
with a perforated lid : the can is weighted at the 
bottom and attached at the lid to a long pole or 
piece of cord. The body of the can is fitted to the 
lid and held firmly by a simple bayonet clip or in 
the same way that incandescent electric lamps are 
fitted to their holders. 

The vessel is lowered into the tank at different 
depths and then slowly raised ; as it is withdrawn 
the semi-liquid rushes in through the perforations 
and a sample is thus obtained. More elaborate 



42 CEMENT CHEMISTS 1 HANDBOOK 

apparatus will be found figured in many English 
and American works on cement manufacture. A 
single sample taken at one depth should never be 
used for analysis. A " grain sampler" will be found 
very useful for sampling dry raw meal or cement. 

Samples of slurry that have been allowed to 
stand, even a short time, must be well shaken 
before examination. 

(41) Moisture. Into a dry and tared flat- 
bottomed porcelain dish weigh out 5 grams of the 
well-mixed slurry, place in a hot air oven or on a 
hot plate at about 110 to 120 C. until quite dry, 
cool in a desiccator and weigh rapidly. 

Loss in weight x 20 = per cent, moisture. 

(42) Remove the dried material from the dish 
with a spatula, powder finely in an agate mortar, 
and place in a stoppered weighing tube. Dried 
slurry very quickly absorbs moisture, so it is better 
to place the powdered material in the oven for a 
short time before bottling. 

(43) Analysis. Ignite 0*5 gram in a platinum 
crucible in the muffle for fifteen to twenty minutes 
at a good red heat. Cool in desiccator and weigh. 

Loss in weight x 200 = loss on ignition. 

(44) Upon the ignited sample carry out the 
analysis as described under Limestone, SiO 2 and 
Insol. (5 and 6) ; Insol. (6); A1 2 O 3 + Fe 2 O 3 (7) ; CaO 
(8) ; and MgO (11) ; CO 2 (14) or (15) ; sulphur and 
sulphates (13) ; and (29) if necessary. 



PROPORTION OF RAW MATERIALS 43 

(45) The excess of the loss on ignition over the 
C0 2 estimated or found by calculation from CaO and 
MgO may be stated as "organic matter" without 
any grave inaccuracy. 

For works routine the following determinations 
are of great importance. Moisture (as in 41). 

(46) " Fineness." Weigh out 100 grams of the 
wet slurry with fair accuracy, wash it with a gentle 
stream of water from the tap into a 180-mesh sieve 
especially kept for the purpose. Continue the 
washing until the water that runs through is quite 
clear. Then wash the residue up together, and 
with a wash bottle transfer it to a small evaporat- 
ing dish ; place upon the hot plate or in an oven, 
and dry. 

Weigh the residue ; calculate the percentage upon 
the dried material thus : 

Weight of residue x 100 = cent finenegs 

per cent, moisture 

With dry meal sift 50 or 100 grams in the usual 
way, using 180-sieve, and weigh the residue: 

Weight x 2 = per cent, residue upon 180. 
It is sometimes useful to estimate the chalk in 
this residue by a rapid method. 

(47) Estimation of CaCO 3 . In most works 
in England this constitutes the greatest part of the 
daily routine, and as the production of a uniform 
article largely depends upon the use of a regular 
raw mixture, too much time and attention cannot 
well be paid to this important item. 



44 CEMENT CHEMISTS' HANDBOOK 

Owing to the use of calcimeters, the actual routine 
determinations can generally be safely carried out 
by untrained assistants who by continual practice 
have become proficient in this part of the laboratory 
work. Constant supervision and occasional " check" 
estimations by the chemist are necessary with even 
the most conscientious workers, in order to keep 
them up to the required standard of speedy 
accuracy. 

There are many good calcimeters on the market, 
all more or less inaccurate ; but when once the error 
is known, if it be constant, the actual accuracy of 
the result is practically unimportant, as the chemist 
in charge should know at what figure to work 
with any given apparatus. Where more than one 
machine is in constant use, they should be so regu- 
lated as to give strictly comparable results. For 
this purpose it is better to prepare a standard raw 
mixture by careful and accurate weighing of the 
raw materials after analysis than to use powdered 
and dry calcite. 

(48) Preparation of a Standard Dry Slurry 
or Raw Meal. Carefully analyse a good sample 
of the ordinary mixture that is known to produce 
the best results in practice. Then dry a small 
sample of each of the raw materials, reduce to the 
necessary fineness, and accurately weigh up and 
carefully mix in the proportions found by analysis 
of raw materials and slurry. 

A stoppered bottle of this should always be kept 
ready for use. When a check analysis is required, 



PROPORTION OF RAW MATERIALS 45 

it is only necessary to dry a little of the standard 
slurry in the air oven at 105 C., and allow it to 
cool in the desiccator. 

(49) Calcimeters may also be standardised, using 
dry pure calcite which has been powdered in an 
agate mortar. With calcimeters upon which it is 
usual to take *5 gram of slurry, it is convenient to 
take only '375 gram of calcite, which should give a 
result equivalent to 75 per cent. CaC0 3 after the 
usual corrections. 

(50) Slater's Calcimeter. This is an instru- 
ment which deserves to be more widely known and 
used than at present. It is fairly simple in con- 
struction, and can readily be adjusted. It requires 
perhaps rather more skilful manipulation than some 
others, owing to the necessary alterations of the 
amounts used at varying temperatures. 

As shown in the illustration, it consists mainly of 
two parts, the outer containing vessel A, and the 
inner bulb and tube B. Upon the leg of this bulb 
are graduations usually running by *5 from 70 to 
80, which are read direct as percentages of CaC0 3 , 
as described later. 

Above the bulb is a zero mark to indicate the 
correct amount of paraffin with which the instru- 
ment has to be filled before use. In the bulb a 
small hydrometer float is placed bearing a scale as 
shown in the enlarged sketch. The markings refer 
to the height of the barometer in millimetres, the 
usual markings commencing at 740 and rising to 



46 CEMENT CHEMISTS 1 HANDBOOK 

780 by 2'5 mm. The top of the instrument is 
closed by a cork, through which passes a thermo- 
meter, dipping well into the mineral oil and keeping 
the bulb in position. The bulb is attached, by a 




FIG. 3. SLATER'S CALCIMETER. 



leading tube of glass and a piece of rubber tubing, 
to the generator bottle (D). The rubber used 
should always be of the same diameter, J inch, and 
length 1 foot, between the ends of the glass tube 
and generator. 



PROPORTION OF RAW MATERIALS 47 

The instrument as sent out generally requires 
standardisation. It is used as follows : 

(1) Take the reading of the barometer in milli- 
metres, and find the nearest corresponding mark on 
the float. 

(2) Take the temperature of the oil in degrees C. 

(3) From the table (27A) ascertain the correct 
weight of material to use in milligrams, and weigh 
this out accurately.. 

(4) Transfer the weighed slurry to the generator 
bottle (D), which must be quite dry. 

(5) Eun from a burette 5 c.c. of dilute commercial 
HC1 (1:1) into the test-tube, attached to the gene- 
rator bottle stopper, by means of the hole in the side. 

(6) Fit the leading tube from calcimeter to the 
bottle, and slip the small piece of rubber over the 
outlet hole. 

(7) Tip the acid on to the slurry and shake well 
to disengage C0 2 . The float will then sink in the 
paraffin, and the mark on the stem which is found 
to correspond with the correct barometer reading on 
the float should be the percentage of CaC0 3 in the 
slurry or material taken. 

The instrument may be adjusted by adding a 
little oil when the reading obtained is high, or vice 
versd. 

By making use of the table given in the Appen- 
dix materials higher in CaCO 3 than 80 per cent, 
may be estimated (2 8 A). 

The following precautions should be observed in 
using this apparatus : 



48 CEMENT CHEMISTS 1 HANDBOOK 

(1) Avoid holding the generator in the hand 
longer than is absolutely necessary, and hold the 
neck and stopper of the bottle. 

(2) See that the rubber is over the outlet hole 
before spilling the acid, and that it is removed 
before disconnecting generator. 

(3) Spill the acid carefully so that none be forced 
up the leading tube. 

Use paraffin that has been placed over CaCl 2 , and 
has such a specific gravity that the hydrometer 
sinks to the red mark on its stem. Use acid of the 
correct strength. 

The Schleibler, Faija, and other calcimeters are 
so well known and have been so frequently described 
and illustrated as not to warrant description here. 
A modification of Schleibler's instrument introduced 
by Mr. H. K. G. Bamber, F.C.S., and much used in 
the A.P.C.M. Works, will be briefly described and 
illustrated (Fig. 4). 

Bamber's Calcimeter. Weigh out accurately 
5 gram of the dried and finely pulverised slurry 
and transfer to generator bottle (14). Eun into 
the gutta-percha tube 8 c.c. of hydrochloric acid 
(sp. gr. 1-125) and place carefully in bottle. Fill 
measuring tubes with water from Woulff's bottle (6), 
or reservoir, until water stands at zero mark on the 
graduated tube. 

Fix stopper to generator bottle and immerse to 
the neck in the running water which fills the lead- 
lined wooden vat, until it is at the same temperature 



PROPORTION OF RAW MATERIALS 49 

as the water in the tubes 2 and 3. This is so when, 
upon opening clip (13), the water in the tubes re- 
mains at the same level. 

Take the generator bottle in the right hand and 




FIG. 4. 



50 CEMENT CHEMISTS 1 HANDBOOK 

cautiously spill the acid in the tube upon the slurry. 
At the same time with the left hand release clip (7), 
shake the bottle vigorously for about half a minute, 
and replace under water in the nest. During the 
evolution of the gas care must be taken to keep the 
level of the water in the plain tube (3) about an inch 
above that in the measuring tube (2). Allow to cool 
for about three minutes, adjust levels of water, and 
take reading. Note temperature of water and also 
barometric pressure. 

To Calculate Percentage of CaCO 3 . To 
calcimeter reading in c.c. add correction for absorp- 
tion of CO 2 by acid. This may be obtained by per- 
forming a check estimation, using Iceland spar or 
standard slurry. The figure usually taken for this 
instrument lies between 3*5 and 4 '2 c.c. By means 
of Table (30 A) Pressure of aqueous vapour in 
Appendix note deduction to be made for given 
temperature from observed barometric pressure. 
Refer to Table (31 A), and under the ascertained 
temperature find the corrected calcimeter reading 
(or nearest) ; in a line with this, denoted by 
heavy type, will be found the reading at C. 
The figure so obtained is now traced on Table 
(32A) under the correct barometric pressure, and 
in a horizontal line will be found in heavy type 
the percentage of CaCO 3 at C. and 760 mm. 
pressure. 

By means of Table (29A) having performed a " loss 
on ignition," the calculated CaC0 3 (54) may be 
obtained. 



PROPORTION OF RAW MATERIALS 51 

(52) Estimation of CaCO 3 by means of 
Standard Acid and Alkali. The following is 
an epitome of a method described by R. K. Meade. 
(Portland Cement, p. 231) : 

Prepare f N HC1 and f N NaOH, and standardise 
against a standard sample of slurry. The method 
of standardisation and working is as follows : 

Weigh 1 gram of sample into a 600-c.c. Erlenmeyer 
flask and run in 50 c.c. of the standard acid. Close 
the flask with a cork bearing a piece of glass tube 
30 in. long and f in. diameter, which acts as an air 
condenser. Heat the flask until steam just begins 
to issue from the upper end of tube. This should 
take about two minutes. Remove from heat and 
rinse the tube down carefully with water, remove 
cork and wash down sides of flask. Add a drop 
or two of 1 in 1000 phenolphthalein or methyl 
orange and titrate with standard alkali until just 
neutral. 

If the standard sample contains L per cent, of 
CaC0 3 and d c.c. of alkali are required, then to find 
percentage of CaC0 3 in other samples it is only 
necessary to subtract the number of c.c. of alkali 
required in their case from d, multiply by two, and 
subtract from L ; if number of c.c. is greater than d, 
subtract d from that number, multiply by two, and 
subtract from L. Each c.c. of exactly f N alkali is 
equivalent to '02 gram or 2 per cent. CaC0 3 ; so 
that, after standardisation, a table may be prepared 
showing percentages of CaCO 3 corresponding to 
different quantities of alkali. It is necessary to 



52 CEMENT CHEMISTS 1 HANDBOOK 

prepare samples to same state of fineness for each 
determination. 

(53) Loss on Ignition, Calculated CaCO 3 
and CaO in Slurry. When using materials con- 
taining organic matter, such as peat, etc., it will 
be found very useful to ascertain the CaC0 3 in the 
meal after allowing for the organic matter present, 
and this may be done as follows. Find the loss 
upon ignition of *5 gram dry slurry or meal as 
in (43). 

Loss in weight x 200 = per cent. C0 2 + H 2 and 
organic matter (A). 

(54) Calculated CaCO 3 . Calculate the CaC0 3 , 
found upon calcimeter, into C0 2 by dividing thus, 

CaCOo x 44 

- 1 ^~ = per cent. C0 2 (B). 

Then, 

Loss upon ignition (A) -- C0 2 (B) = organic 

matter (C). 

And 100 -- organic matter (C) = parts of 
material in which the CaC0 3 exists after removing 
the organic matter by ignition (D). 
Thus, 

per cent. CaCOo found x 100 

j) - = calculated CaC0 3 . 

The actual calculations only take a few seconds 
if the tables in Appendix be used. 

(55) The residue obtained after ignition should be 
reserved and the CaO present determined by the 
rapid method as described in chapter v. (132); 



PROPORTION OF RAW MATERIALS 53 

after allowing for the loss upon ignition the CaO 
found should be approximately the same as the 
clinker made from this slurry will contain. Owing 
to various circumstances, this is not always quite 
the case in practice, but this serves as an excellent 
check upon the calcimeter or other determinations. 
The calculation is as follows : 

Per cent, lime in slurry x 100 

100 -loss. = calculated CaO. 

(56) Control and Alteration of the Raw 
Mixture. Owing to the various systems in vogue 
on different works, it is impossible to lay down any 
hard and fast rules for the control and regulation 
of the slurry or raw meal. The growth of the cement 
industry in this and other countries has brought 
about the successful use of raw materials differing 
so widely in composition as to require in some cases 
plant and methods of working of quite a distinct 
and special character. Before finally deciding upon 
a method of working, the chemist in charge should 
assure himself that the routine proposed fulfils the 
following requirements : 

(1) That there is a regular supply of raw material 
sufficient to keep the mills and kilns going con- 
tinuously. 

(2) That the unit loads of materials are of con- 
stant weight or bulk. 

(3) That it is possible to readily obtain a sample 
of either raw material being used at any moment for 
check analysis. 



54 CEMENT CHEMISTS 1 HANDBOOK 

(4) That accurate returns of the quantity of 
material used be sent to the laboratory at stated 
periods, in order that any deviation from the working 
instructions may be at once noted. It is absolutely 
essential that a responsible person be in charge of 
each mill and be made answerable for any irregu- 
larity of working either in the feeding or output. 

In regard to alteration of the feed of raw 
materials, it will generally be found most con- 
venient to keep the clay or argillaceous supply 
constant, and to vary the chalk or limestone. 

The importance of being able to obtain an average 
sample of the slurry or raw meal for routine 
analysis has already been mentioned. In order 
that this work be not interfered with, the samples 
should be fetched by a laboratory assistant, marked 
for reference; and immediately examined. All re- 
sults should be carefully entered up for future 
reference. 

Before making an alteration in the raw supply at 
any mill, the cause of the erratic behaviour should, 
as far as possible, be ascertained and noted ; then 
the desirability of making a temporary or permanent 
alteration will at once be known and acted upon. 
Time should be given for the alteration to have 
effect before again checking the output. It is un- 
wise to irritate the mill hands by useless and 
vexatious alterations and orders. 

In working upon the dry system it is best to 
keep a silo full of limestone or clay, and work so 
as always to require adjustment in one direction, 



PROPORTION OF RAW MATERIALS 55 

For this purpose, either wet or dry process, it is 
well to have three tanks or silos for the raw meal : 
one to run the make into, one that may be tested 
and corrected, and one containing material of the 
correct composition. It should be impossible for 
the kiln attendants to use any material but that 
passed for use by, the chemist in charge ; even then 
the meal, as fed into the kilns, should be regularly 
sampled, checked, and the results entered in the 
laboratory records. In a word, too much care 
cannot well be given to this branch of the laboratory 
work. 



CHAPTER IV 

ANALYSIS OF FUEL, LUBRICANTS, 
WATER, AND KILN GASES 

THE fuel used chiefly on a cement works is coal or 
coke. Brief descriptions only are given of the 
chief methods of analysis ; for fuller description, 
especially of the calorific value determination, the 
inexperienced reader is recommended to consult 
larger works. 

(57) COAL. In order to obtain an average 
sample of the fuel, it is best to have a part of the 
freight set apart as it is being unloaded, say one 
barrow or grab full in ten, then have this well 
mixed and reduced to a convenient bulk by the 
method of quartering. When sampling a large 
cargo it will be found advisable to obtain several 
samples and carry out check assays. 

When not too large, the whole of the sample 
brought to the laboratory should be coarsely 
powdered and quartered, and the portion selected 
for analysis all ground to pass at least the 90 in. -mesh 
sieve must be reserved in a well- stoppered bottle 
or jar. 

56 



ANALYSIS OF FUEL, ETC. 57 

(58) Moisture. It is well to estimate the 
moisture as soon after receiving the sample as 
possible. 

Weigh into a weighed platinum capsule '5 or 1 
gram of the powdered coal and heat in an air oven 
at 105 C. for not more than one hour. Cool in a 
desiccator and weigh rapidly, as dry coal is very 
hygroscopic. 

Loss in weight x 200 (or 100) = per cent, 
moisture at 105. 

Epitome. 
"5 gram in oven at 105 0. for one hour. 

(59) Ash. Gently ignite the dried coal over a 
bunsen burner or in the muffle, first at a low tem- 
perature, until all the carbonaceous matter has 
burnt off. The colour of the ash sometimes indicates 
its nature. 

Cool in a desiccator and weigh. 
Total weight weight of capsule x 200 = per cent, 
ash. 

Epitome. 
'5 gram ignited in muffle. 

(60) Volatile Matter. One gram of the sample 
is placed in a large weighed platinum crucible 
having a well-fitting cover. Heat the crucible with 
lid on for two minutes over a bunsen burner, or 
until no inflammable vapours are emitted, and then 



58 CEMENT CHEMISTS 1 HANDBOOK 

for a further period of three minutes over a blast 
burner. Allow to cool in a desiccator, and weigh. 

Loss in weight x 100 = volatile matter + moisture 
per cent. 

Epitome. 

One gram heated in closed crucible for two 
minutes over bunsen, + three minutes over 
blast burner. 

In order to obtain concordant and comparable 
results, it is necessary always to perform this opera- 
tion in exactly the same manner. 

The per cent, moisture (56) subtracted from 
volatile matter + moisture will give the volatile 
matter. 

(61) " Fixed carbon," or better, fixed carbon- 
aceous residue. This is obtained by difference. 

100 - per cent, (moisture + volatile matter + ash) = 
" fixed carbon." 

(62) Coke. This is not, as a rule, of great 
importance. The residue left after the determina- 
tion of the volatile matter is, roughly speaking, 
coke. It should be tested to see whether it is 
friable or compact. 

Coke may be more accurately determined by 
placing 1 gram in a covered porcelain crucible placed 
in a large Battersea round crucible and surrounded 
and packed well in and covered with powdered 
charcoal. 



ANALYSIS OF FUEL, ETC. 59 

The lid of the large pot is luted on with clay, and 
the whole dried and heated in a wind or gas furnace 
until it is thoroughly hot. 

After being allowed to cool, the porcelain crucible 
and lid is carefully removed, and the coke brushed 
out on to a watch glass and weighed. 

Weight of coke x 100 = per cent. coke. 

Epitome. 
One gram heated in covered crucible in furnace. 

(63) Sulphur. Mix 1 or 2 grams of the finely- 
powdered coal with twice its weight of a mixture 
consisting of 1 part dry K 2 C0 3 and 2 parts MgO 
in a capacious platinum crucible and cover with a 
little more of the fusion mixture ; place in muffle at a 
red heat for half an hour, remove, allow to cool, 
dissolve and acidulate with E HC1, evaporate to dry- 
ness, take up with 10 c.c. of 10E HC1 and a little 
water, filter off Si0 2 ; dilute filtrate somewhat, and 
estimate S as BaS0 4 (13). 

Epitome. 

Fuse 1 or 2 grams with K 2 C0 3 and MgO mix- 
ture. 

Dissolve in hydrochloric acid, remove Si0 2 . 
Ppt. with barium chloride solution (13). 

(64) Analysis of Ash. Ignite 10 grams or 
more of the fuel in a platinum capsule until free 
from carbonaceous material. Use of this 1 gram or 



60 CEMENT CHEMISTS 1 HANDBOOK 

more, and determine SiO 2 , A1 2 O 3 , Fe 2 O 3 , CaO, and 
MgO after fusion, as in (17) ; and, if necessary, upon 
other portions S0 3 (30) and P 2 5 (39). 

(65) ANALYSIS OF COKE. The methods 
described under Coal may be used for the determi- 
nation of moisture (58), ash (59), volatile matter 
and fixed carbon (60) and (61), and sulphur (63). 

A mixture of MnC0 3 and Na 2 C0 3 may be used 
(Neilson's method, Chemical Neivs, April 24, 1891, or 
Phillips, p. 125), instead of the mixture used in (63). 

(66) CALORIFIC POWER OF FUEL. 

For this determination a calorimeter is required. 
One of the simplest is Lewis Thompson's ; but one of 
the improved forms of this instrument using oxygen 
gas and having electric ignition is more accurate 
and satisfactory. 

In the ordinary form a known weight (2 grams) of 
the fuel is mixed with sufficient finely-powdered 
ignition mixture (KC10 3 3 parts, KN0 3 1 part), 
placed in the copper cylinder and ignited, when all 
is ready, by means of a fuse. 

The cylinder and attachment is immediately 
plunged into 2000 c.c. of water at a known tempera- 
ture contained in the special vessel. After combus- 
tion the increase of temperature is noted. For 
details consult Beringer, Phillips, or the instructions 
given with the instrument. 

In the improved forms the coal is made into a 
pellet and ignited whilst under the water by mjeans 
of an electric current. 



ANALYSIS OF FUEL, ETC. 61 

As a rule each instrument requires the use of 
special factors or corrections, but in every case the 
result is expressed as calories or the number of units 
required to raise one unit of water through 1 C. ; 
generally 1 gram is the unit used. The British 
Thermal Unit is Ibs. of water raised 1 F. by 1 Ib. 
of fuel. 

.-. Calories x.J'i B.T.U. 

_ calories 
and p-o = evaporative power. 



537 being the latent heat of steam. 

For use in rotary kilns the character of the coal 
when burning is of greater importance than the 
actual calorific power. 

(67) Fineness. This is determined in the same 
way as with cement, the 100-sieve being used. To 
obtain good results in a rotary kiln the residue should 
not exceed 5 per cent., the coal should be quite dry 
and low in ash, and easily combustible. 

The methods given above can be used for any class 
of coal, but it is desirable to use a rather higher 
temperature or heat for a longer period to estimate 
the volatile matter in anthracite or steam coal. 

Concerning the classification of coals, " Analysis 
of British Coals," Colliery Guardian, may be con- 
sulted. 

LUBRICANTS. The chief methods of exami- 
nation only can be mentioned . If much important 



62 CEMENT CHEMISTS 1 HANDBOOK 

work has to be done the chemist is recommended to 
consult Lewkowitsch's or other large work. 

Lubricants may be very roughly divided into three 
classes solid, semi-solid, and liquid. Only grease, 
fats, or oils will be here dealt with, but it may be 
mentioned that graphite, mineral, and compound 
lubricants should be free from grit, acid, and alkaline 
bodies or substances likely to decompose and produce 
acids, &c. 

Before reporting on a lubricant it is necessary to 
know for what purpose it is intended to be used. 
The following tests may be considered essential : 

(68) Loss or Gain in Weight on Exposure. 
Into a weighed watch-glass place 1 gram of the oil, 
and expose in an air or water bath at 100 C. for 
twelve hours. Allow to cool in a desiccator and 
weigh. 

Loss (or gain) in weight x 100 = percentage loss 
(or gain). 

Good mineral oils rarely lose more than 1 per 
cent. ; some vegetable oils increase in weight owing 
to oxidation. The residue should not exhibit any 
sticky or gummy properties. 

Epitome. 
1 gram at 100 for twelve hours. 

(69) Specific Gravity. The sp. gr. of oils, 
liquid at 15, may be fairly accurately determined 
by the hydrometer or Westphal balance. 



ANALYSIS OF FUEL, ETC. 63 

A specific gravity bottle may be used for any oil 
or fat at any temperature. Weigh the bottle with 
thermometer stopper, which should be pierced or 
have a file mark cut to allow excess of oil to escape. 
Fill with previously boiled distilled water at the 
temperature to be used. Dry perfectly ; cool and 
weigh. The water content of the bottle will thus 
be known (A). 

By means of a tube or pipette carefully fill the 
perfectly dry bottle with oil or molten fat, which 
should be at a slightly lower temperature than that 
at which the determination is to be made. Raise 
to the required temperature. 

Carefully wipe off excess, allow to cool, and 
weigh (B). 

Weight of oil (B) 

o _ \ / _ - 



Weight of water (A) at same temperature 
gravity at stated temperature. 

A convenient method to obtain the desired tem- 
perature is to place the bottle in a small jar or 
copper vessel on a hot-air oven. 

(70) Viscosity. This is best determined in a 
standardised Redwood viscosimeter. The viscosity 
of an oil varies with the temperature at which it is 
determined. According to Phillips, for ordinary 
machinery it should be determined at 15, 30, and 
60 C. ; and for cylinder oil at 100, 120, and 150 0. 
In order to obtain the viscosity of an oil, it is heated 
in an air bath to the required temperature, and 
poured into the apparatus up to the point of the 



64 CEMENT CHEMISTS' HANDBOOK 

gauge. The outer vessel, which may be filled with 
water, oil, or any other convenient liquid, is then 
warmed until both it and the oil to be tested are at 
the required temperature. A plug is then removed 
and exactly 50 c.c. of oil allowed to runout, and the 
time taken in seconds noted by means of a stop 
watch. For comparative results consult tables pub- 
lished by Redwood and others. 

(71) Flash-Point. This may readily be ascer- 
tained with Abel's flash-point apparatus. With a 
little practice the principles of the determination 
can soon be mastered. Full instructions are gene- 
rally sold with the apparatus, or can be found in 
the Petroleum Acts or any work on oil analysis. 
For oils flashing above 100 C. the air bath is heated 
by means of a small bunsen burner or spirit lamp. 
The flash-point of an oil should be higher than the 
temperature that will be obtained during work. 

(72) Free Mineral Acids. Shake up 50 grams 
of the oil with sufficient distilled water in a stop- 
pered flask or bottle, and allow to stand for some 
time; then separate the oil by means of a separating 
funnel. To the aqueous extract add a drop of 
methyl orange solution ; a pink colouration will indi- 
cate the presence of free mineral acid. If sufficient 
in amount, . titrate back to the neutral tint with 

- or - NaOH. The nature of the acid must be 
10 100 

determined by a qualitative analysis of the extract. 
H 2 S0 4 is the acid most frequently found. 



ANALYSIS OF FUEL, ETC. 65 

Epitome. 

Agitate 50 grams of oil with distilled water. 
Separate, add methyl orange, and titrate with 

N N M nTT 

10 r Too Na01L 

(73) Free Fatty Acid. Weigh out 50 grams 
of the oil into a flask, and add 100 c.c. methylated 
spirit rendered just slightly pink by the addition of 
a drop or two of phenolphthalein and one drop of 
E NaOH. Shake up together well. If free fatty 
acid be present the solution will become colourless. 

N 
Titrate with standard NaOH until a permanent 

pink colouration is obtained. 

N 
One c.c. of NaOH = '0282 gramoleic, '0256 gram 

palmitic, or *0284 gram of stearic acid. 
With palm oil use only 5 grams. 

Epitome. 

Agitate 50 grams of oil with alcohol and phenol- 
phthalein solution. 
Titrate with standard alkali. 

(74) Separation of Fatty and Mineral Oils. 

Saponification equivalent. Weigh out 2*5 grams 
of the oil into a strong flask or bottle ; add 25 c.c. of 

- standard alcoholic KOH. Place the flask, with 

M 



66 CEMENT CHEMISTS 1 HANDBOOK 

the stopper loosely fitted, in a bath of cold water 
and cause to boil. As soon as the contents of the 
flask are seen to boil, fix the stopper in tightly and 
wire it down ; replace in the bath, cause the water 
to boil, and allow the flask to remain for about half 
an hour, with occasional shaking. Remove from 
bath and allow to cool ; remove stopper and titrate 

excess of KOH by means of HC1, using phenol- 

2i 

phthalein as indicator. 

A blank experiment is conducted at the same 
time, and thus the exact strength of the alcoholic 
KOH is ascertained and the amount absorbed by 
the oil calculated. 

The mean percentage of KOH absorbed by the 
chief fatty oils has been found to be 20*08 per cent. ; 
therefore 4*98 parts of fatty oil are saponified by 1 
part of KOH. Then number of c.c. neutralised by 
oil x 40 x 4'98 x '02805 = approx. per cent, of 
fatty oil. 

The saponification equivalent is the number of 
grams of oil decomposed by one litre of a normal 
alkali (KOH or NaOH solution) ; therefore 

2*5 x 2000 

-^P 1 = sap. value. 

No. of c.c. 

Epitome. 
Saponify 2'5 grams of oil with 25 c.c. of 

^ KOH. 
Titrate excess with HC1. 



ANALYSIS OF FUEL, ETC. 67 

WATER ANALYSIS. The examination of 
a water on a works is usually undertaken to ascer- 
tain the suitability for use in boilers, &c., rather 
than to judge of its fitness for drinking and domestic 
purposes. As a matter of fact, a works laboratory 
is rarely suitably equipped or circumstanced to 
permit of such an analysis being conducted with any 
hope of obtaining reliable results. The processes 
necessary to judge of the suitability of water for 
drinking purposes are therefore only very briefly 
described. 

(75) Collection of Samples. Clear glass Win- 
chester quart bottles are very suitable for collecting 
arid storing water samples. Before being filled with 
the water to be tested, they should be thoroughly 
washed until free from all traces of acid, ammonia, 
&c., that they may have contained. Bottles which 
have been used for acids should be preferred. Before 
filling, the bottles should be washed out well with 
the water under examination ; the stopper should 
be fastened firmly down with string or wire, and 
sealed. It is well to take and keep sealed bottles 
of the works water-supply, should there be any 
possibility of future contamination by neighbouring 
manufactories. Samples of the works outflow and 
waste waters should also be kept. 

(76) Colour, Odour, Reaction. The colour 
can be judged by looking down through a tall glass 
cylinder full of the water; tint or turbidity, if any, 
should be noted. Odour should be observed ; this 



68 CEMENT CHEMISTS 1 HANDBOOK 

will be more noticeable when the water is gently 
warmed, or half a litre of it well shaken in a wide- 
mouthed litre flask. 

The reaction should be tested by means of a strip 
of neutral litmus paper ; some waters give naturally 
a slight alkaline reaction. Acidity would most 
likely be due to contamination with chemical or 
other works waste, although it is sometimes caused 
by carbonic acid in solution, which will disappear 
upon boiling. Waters passing through a peaty soil 
may also give an acid reaction. 

(77) Sediment and Suspended Matter. 
The character of any sediment or suspended matter 
should be noted. If necessary a little may be with- 
drawn by means of a glass tube and examined under 
the microscope. 

The sediment should be well searched for the 
lower forms of diatom acere and algse, some of 
which cause a water to smell as if contaminated 
with dead fish. 

Any great amount of suspended matter may be 
estimated by filtration of one or two litres of the 
water through a tared filter. The filter and contents 
are dried at 100 C. and weighed. 

Increase in weight = suspended matter per litre. 

The inorganic matter in suspension may be 
estimated by igniting the filter and contents in a 
crucible ; recarbonate by adding a drop of ammonium 
carbonate, and ignite again at a low temperature 
and weigh. 



ANALYSIS OF FUEL, ETC. 69 

Weight ash of filter = insoluble mineral matter 
per litre. 

Epitome. 
Filter 1000 c.c. through tared paper and weigh. 

Before proceeding with the chemical analysis it 
is well to ascertain whether to report as grains per 
gallon or parts per 100,000. Most engineers will 
probably prefer results in grains per gallon. It is 
really unimportant, if the report is to be used by 
intelligent men, as it is only necessary to multiply 
grains per gallon by ten and divide by seven or 
vice versa with parts per 100,000 to convert one into 
the other. 

(78) Total Solids. Evaporate 250 c.c. of the 
water to dryness in a clean dry platinum or porcelain 
weighed evaporating basin, at first over an argand 
or bunsen burner, and finally on the water bath. 
Allow to cool in a good desiccator and weigh 
rapidly, as the solids are often very hygroscopic. 

Weight - weight of dish x 400 = parts per 100,000. 

Epitome. 
Evaporate 250 c.c. to dryness and weigh. 

(79) A qualitative examination may be made of 
the solids ; if a quantitative analysis is required it 
will be necessary to evaporate 1000 c.c. or more 
of the water to dryness. Estimate SiO 2 , A1 2 O 3 , 
Fe 2 O 3 , P 2 O 5 , CaO, MgO, CO 2 , SO 3 , as in ordinary 



70 CEMENT CHEMISTS' HANDBOOK 

analysis. (See paragraphs Nos. 5, 7, 8, 9, 11, 13, 14, 
39.) NaCl will be found separately. Na and K may 
be estimated or reported by difference. The chief 
constituents are CaCO 3 , CaS0 4 , MgC0 3 , MgSO 4 , 
and organic matter in solution in the case of peaty 
waters. 

(80) Chlorine as Chlorides. A standard solu- 
tion of silver nitrate containing 4790 grams per 
litre will be required ; also a dilute solution of 
potassium chromate free from chloride. Measure 
100 c.c. of the water to be tested into a clean flask 
and add a drop or two of the chromate solution. 
Run in the standard silver nitrate solution until a 
permanent orange tint is obtained. To ascertain 
the end point needs some little practice, and results 
should always be duplicated. 

Read off from the burette the number of c.c. of 
silver nitrate used. 

Number of c.c. = parts per 100,000 of 01. 
Chlorine x l'65 = parts per 100,000 of NaCl. 

Epitome. 

Titrate 100 c.c. with standard silver nitrate, 
using potassium chromate as indicator. 

(81) Hardness. The hardness of a water is a 
factor of great importance on a works. Hardness 
is divided into two classes : " permanent," mainly 
due to sulphates of calcium and magnesium (and the 
other alkaline earths) ; and " temporary," due to 



UNIVERSITY 



ANALYSIS OF FUEL, ETC. 71 

the carbonates of these metals, the latter being 
removable by boiling. 

(82) Estimation of hardness by standard soap 
solution. The following standard solutions are re- 
quired. Standard hard water made by dissolving 
without loss 0*2 gram of powdered calcite (CaCO 3 ) 
in dilute hydrochloric acid and evaporating to dry- 
ness on the water bath several times until quite 
free from acid. The Ca01 2 is then dissolved and 
made up to 1000 c.c. with pure distilled water. 

One c.c. = "0002 gram of CaCO 3 or 20 parts per 
100,000. 

(83) Standard Soap Solution. A standard 
potassium oleate soap solution may be readily pre- 
pared by dissolving 80 grams of pure oleic acid in 
" proof " spirit and exactly neutralising wilh alcoholic 
potassium hydrate solution, using a drop or two of 
phenolphthalein as indicator. The solution is then 
titrated with the standard hard water (82). 

(84) Standardisation of the Soap Solution. 
Measure 100 c.c. of standard hard water into a 
clean glass-stoppered bottle, and run the soap solu- 
tion into the bottle a few c.c. at a time until a 
lather begins to form ; then add the soap solution 
more cautiously, inserting the stopper and shaking 
between each addition. When the reaction is near- 
ing completion the contents of the bottle will only 
give a faint dull sound. Soap solution must be 
added until a permanent lather, which persists for 



72 CEMENT CHEMISTS' HANDBOOK 

at least two minutes, is obtained. The soap solution 
must be then so diluted that the 100 c.c. of water 
require exactly 21 c.c. to produce a lather, the extra 
c.c. being required to produce a lather with 100 c.c. 
of distilled water. 

Suppose the water only requires 16 c.c. of soap, 
then every 16 c.c. of the solution must be diluted 
with a mixture of about 2 to 1 alcohol and water to 
make 21 c.c. Rectified spirit or methylated spirit 
dehydrated over lime and redistilled must be used, 
as ordinary methylated spirit produces a ppt. with 
water. 

One c.c. of the standard soap solution will thus = 1 
of hardness or 1 part of CaC0 3 per 100,000. If 70 
c.c. of water are taken, results as expressed in degrees 
on Clarke's scale will be obtained, i.e., 1=1 grain 
of CaC0 3 per gallon. 

(85) To ascertain temporary and permanent 
hardness of a water. Measure 100 c.c. of the water 
under examination into the titration bottle ; or, if 
the water is known to be very hard, take 50 c.c. 
and dilute with distilled water. Run in the soap 
solution cautiously as described until a permanent 
lather is obtained ; deduct 1 c.c. from the amount 
used ; then number of c.c. = degrees of total 
hardness. 

Epitome. 

Titrate 100 c.c. with standard soap. 

(86) Permanent hardness. Boil, in a flask or 
beaker, 100 c.c. of the water down to a volume of 



ANALYSIS OP FUEL, ETC. 73 

about 50 c.c. or rather less. Allow to cool, filter or 
decant, and make up to 100 c.c. again. Titrate 
with soap solution as before. 

No. of c.c. = degrees of permanent hardness. 

Total permanent = temporary hardness. 

Epitome. 

Titrate 100 c.c., after boiling, with standard 
soap. 

(87) Estimation of hardness by Standard Acid 
temporary. To 500 c.c. of the water, or less if 
very hard, tinted with methyl orange, run in from a 

N 
burette H 2 SO 4 until a red colouration is just 

produced. 

Number of c.c. used = parts per 100,000 of 
CaC0 3 as " temporary hardness." 
Permanent hardness. To 250 c.c. of the 
N 
10 

about half an hour, or, if magnesium salts be 
present, evaporate to dryness. 

Filter off the ppt., or extract the residue with 
boiled distilled water, filter and wash ; when cool, 
make the filtrate up to 250 c.c. 

N . 
Titrate 50 c.c. of the filtrate with -T-Q H 2 S0 4 , using 

methyl orange as indicator. 

N 
Since 10 c.c. of T NaCO 3 was present in every 50 



water add 50 c.c. of TT, Na 2 C0 3 solution and boil for 



74 CEMENT CHEMISTS' HANDBOOK 

c.c. of water, then 10 number of c.c. of acid used = 
number of c.c. of soda removed. Call this x ; then 
soda used by the 250 c.c. of water = (x x 5) ; as 1 c.c. 

N 
of TQ Na 2 CO 3 = -005 gram of CaC0 3 , then (x x 5) x 

005 x 400 = parts of CaCO 3 per 100,000 present as 
permanent hardness. 

(89) Estimation of hardness in a softened water 
or water containing soda. In a water that gives 
an alkaline reaction to litmus or methyl orange there 
can be no permanent hardness, as carbonates of cal- 
cium and magnesium will be pptd. on boiling. Boil 
250 c.c. or 500 c.c. of the water, filter off ppt., if any, 
wash and make up filtrate to original bulk, titrate 

N 
whole or aliquot part of the solution with ^H 2 SO 4 , 

and calculate to Na 2 C0 3 parts per 100,000. 

Number of c.c. of acid used x 200 (or 400) x 
0053 = parts per 100,000 Na 2 C0 3 . 

Contamination. To ascertain whether water 
is contaminated with sewage or with the products 
of animal or vegetable decomposition, it is necessary 
to estimate the free or saline ammonia, and the 
albuminoid ammonia which is derived from nitro- 
genous matter, by boiling with alkaline permanga- 
nate of potassium. 

The following special reagents are required. For 
full particulars of the process involved a work on 
water analysis should be consulted. 

The estimation must be conducted under conditions 



ANALYSIS OF FUEL, ETC. 75 

that admit of no contamination from fumes of am- 
monia, &c. The apparatus and distilled water used 
must also be quite free from any traces of ammonia 
or ammonium salts. 

(go) Standard Ammonium CJiloride. Dissolve 
3*137 grams of pure ammonium chloride in ammonia- 
free distilled water, make up to 1 litre and label as 
"stock NH 4 C1 solution." 

Take 10 c.c. of (90) and dilute to 1000 c.c. 
1 c.c. = -00001 gram of NH 3 . 

(91) Nesslers Reagent. Dissolve 35 grams of 
potassium iodide in about 250 c.c. of distilled water. 
Then add gradually a cold saturated solution of 
mercuric chloride, stirring constantly until a faint 
permanent ppt. is formed ; allow to stand and decant 
off. Then add a cool solution made by dissolving 
150 grams of caustic potash in 150 c.c. of water. Add 
a drop or two of mercuric chloride solution until a 
slight ppt. is formed. Dilute to 1 litre and allow to 
stand. Decant off a portion into a smaller bottle for 
use, and always use a pipette or graduated tube to 
measure out the required quantity of solution. 

(92) Alkaline Permanganate. Dissolve 200 grams 
of caustic potash in about 800 c.c. of ammonia-free 
distilled water. Then add 8 grams of potassium per- 
manganate, allow this to dissolve and boil for a short 
time ; when cool, make up to 1 litre. 

(93) Estimation of "Free A mmonia." -- Distil 
250 c.c. of the water, or less if very contaminated, 



76 CEMENT CHEMISTS' HANDBOOK 

using a large flask fitted to a Liebig's condenser in 
the usual way. The apparatus must first be well 
cleaned and boiled out with ammonia-free water 
until the distillate gives no reaction with Nessler's 
reagent. The distillate from the water under exami- 
nation is collected in a series of Nessler tubes, and 
the operation continued as long as a colouration is 
produced with 2 c.c. of the reagent (91). 

Usually three cylinders are sufficient. To each 
add 2 c.c. of the reagent and prepare a similar tube 
using distilled water ; measure into it 1 c.c., or more, of 
the standard ammonium chloride and then add 2 c.c. 
of Nessler reagent. Tubes are thus prepared to match 
the tint of each tube of distillate, and the total number 
of c.c. of standard ammonium chloride required 
noted. 

Number of c.c. used x '00001 x 400 = parts of 
free ammonia per 100,000. 

The Nessler reagent must always be added to the 
ammonium chloride and not vice versd. Instead of a 
flask and Liebig's condenser a large retort fitted to a 
spherical condenser placed in a bath of water may 
be used. Quite 100 c.c. of distillate is collected and 
tested against standard ammonium chloride as de- 
scribed. 

Epitome. 

Distil 250 c.c. of water. 

Test distillate with Nessler reagent (91). 

(94) Albuminoid Ammonia. To the water re- 
maining in flask or retort add 25 c.c. of the alkaline 



ANALYSIS OF FUEL, ETC. 77 

permanganate (92) and continue the distillation as 
long as possible. Then test the distillate as before, 
and ascertain number of c.c. of ammonium chloride 
solution required to match depth of tint. The 
calculation is the same as above. 

Epitome. 

Add 25 c.c. of alkaline permanganate and re- 
distil. 

For interpretation of results consult a work on water 
analysis. See Appendix 33 A for typical analyses. 

(95) Estimation of Oxygen required to oxidise 
Organic Matter. A standard solution of potassium 
permanganate is required containing 0'395 gram 
per litre. Then 1 c.c. = *0001 gram of oxygen. 

Into a clean glass bottle or flask place 250 c.c. of 
water to be tested ; then add, from a graduated 
pipette or tube, 1 c.c. of the standard permanganate 
solution and about 10 c.c. of dilute sulphuric acid, 
to which has been added enough permanganate to 
make it slightly pink. Allow to stand for fifteen 
minutes at 15 C. If the pink colouration remains, 
the oxygen absorbed is nil ; if it disappears, add 
another c.c. and continue until the colouration is 
permanent for one hour. 

If the water is likely to use a lot of perman- 
ganate solution, take 250 c.c. in flask as before, and 
250 c.c. of distilled water in another flask; add 
10 c.c. of permanganate and 10 c.c. of the dilute 
acid to each, and allow to stand for three hours 



78 CEMENT CHEMISTS 1 HANDBOOK 

at the same temperature (15 0.). Then add a drop 
or two of potassium iodide solution to the distilled 
water as " check," and titrate with a solution of 
sodium thiosulphate containing 1 gram per 1000 c.c., 
using freshly made starch solution as indicator. 
Note the number of c.c. of thiosulphate required to 
just remove the blue colour caused by the iodide 
and starch. Repeat the titration in a similar way 
with the water under examination. 

Note number of c.c. of thiosulphate used. As 
the distilled water uses up no permanganate, the 
equivalent in terms of thiosulphate will be known. 

(96) Estimation of Nitrates + Nitrites. The 
total solids from 500 c.c. of water are taken up with 
a small quantity of distilled water, filtered, and 
washed. The filtrate, after being evaporated to about 
2 c.c., is put into the cup of a nitrometer and then 
carefully into the instrument, which must be full 
of clean mercury. The beaker and cup are then 
washed with a little water which is also allowed to 
run into the graduated tube ; 6 c.c. of 36E H 2 S0 4 
free from nitrates are then carefully admitted, care 
being taken not to admit air. Any air or C0 2 
bubbles which may be produced are carefully driven 
out by raising the other limb of the instrument. 
The tap is again turned off, and the tube and 
contents carefully but thoroughly shaken for about 
ten minutes, or until there is no further increase in 
the volume of gas collected. Allow to cool, and 
then adjust the level of the mercury in both tubes 



ANALYSIS OF FUEL, ETC. 79 

until that in the open tube is about one-tenth of the 
volume of the liquid above the mercury in the 
closed tube. Bead off the volume of nitric oxide 
(NO) and note temperature and barometric pres- 
sure. 

Calculate to volume at 0, and 760 mm. NO 
contains half its volume of nitrogen, so the gas thus 
found represents nitrogen in 1000 parts. 1 c.c. of 
nitrogen weighs -0012544 gram, therefore : 

1 c.c. of N (at NTP) x -12544 = parts of N per 
100,000. 

NX 4-5 = HN0 3 . 

(97) Estimation of Nitrates using Standard 
Indigo Solution. 

The following standard solutions are required : 

Indigo Solution. Digest 1 gram of pure solid 
indigo with 10 c.c. of fuming sulphuric acid for 
several hours on a water bath until all is dissolved. 
Make the solution up to a volume of two litres with 
distilled water. 

Standard Nitrate. Dissolve 1'603 grams of pure 
KNO 3 in one litre of distilled water. This contains 
the equivalent of 1 gram per litre of HN0 3 ; for use 
dilute ten times ; then 

1000 c.c. = O'l gram HNO 3 . 

To standardise Indigo. Take 10 c.c. of the 
dilute nitrate solution and 10 c.c. of distilled water 
in a flask, add 20 c.c. of pure 36E H 2 S0 4 free from 
nitrates, and immediately run in from a previously 



80 CEMENT CHEMISTS 1 HANDBOOK 

filled burette the indigo solution, a few drops at a 
time, until the first brown tint begins to become 
darker, when the addition may be hastened. The 
reaction is complete when the solution assumes a 
decidedly green tint, which is best seen upon dilu- 
tion. With a little practice the end tint is soon 
recognised. 

-r y = strength of indigo per c.c. 

No. ot c.c. used 

To estimate Nitrate in Water. Take 20 c.c. of 
the water and 20 c.c. of 36E H 2 SO 4 and titrate as 
described. If the water contains more than 10 
parts of HN0 3 per 100,000, use 10 c.c. and dilute to 
20 c.c. with distilled water. 

No. of c.c. used x factor x 50,000 = parts per 
100,000 of HN0 3 . 

The indigo should occasionally be checked, as it 
deteriorates after a time. An estimation can be 
carried out in less than five minutes. 

(98) Poisonous Metals. A drinking water should 
always be tested for lead, copper, etc., by passing 
H 2 S gas through a quantity of the water contained 
in a clear glass vessel. No dark colour should be 
produced. If present, lead may be estimated by 
evaporating several litres of the water to a small 
bulk, acidifying slightly with hydrochloric acid and 
ppt. with H 2 S. 

Filter, wash, convert into PbS0 4 , and weigh ; or 
lead may be estimated colorimetricaliy by comparison 
of the depth of tint produced by adding H 2 S to 



ANALYSIS OF FUEL, ETC. 81 

a known amount of water, and also to a standard 
dilute solution of lead nitrate. 

Epitome. 

Pass H 2 S through at least 1 litre of water. 
Estimate as PbSO 4 or colorirnetrically. 

Water softening. Many systems of water 
softening are in vogue ; they are nearly all based 
upon the removal of carbon dioxide and consequent 
precipitation of calcium carbonate by means of lime, 
or precipitation of carbonate and sulphates by means 
of soda ash (Na 2 C0 3 ) or caustic soda (NaOH). 

The following are the principal reactions in- 
volved : 

(1) CaC0 3 + C0 2 + Ca(OH) 2 = 2CaCO 3 + H 2 

(2) MgC0 3 + C0 2 + 2Ca(OH) 9 = 

2CaC0 3 + Mg(OH) 2 + H 2 O 

(3) CaS0 4 + Na 2 CO 3 = CaCO 3 + Na 2 SO 4 

(4) MgS0 4 + Ca(OH) 2 + Na 2 C0 3 = 

CaC0 3 + Mg(OH) 2 + Na 2 S0 4 

(5) CaC0 3 + 2NaOH = Ca(OH) 2 + Na 2 CO 3 

(6) CaSO 4 + 2NaOH = Ca(OH) 2 + Na 2 SO 4 

The following illustrates the method of calcu- 
lating the amount of lime required per 1000 gallons, 
the CaC0 3 present being known from the temporary 
hardness or by analysis of the total solids : 

CaCO 3 + CO 2 + CaO = 2CaCO 3 
100 + 56 



82 CEMENT CHEMISTS' HANDBOOK 

100 parts of CaCO 3 requires 56 parts of quick- 
lime (CaO). 

The water has say 15 parts of CaCO 3 per 100,000. 
1000 parts of water contain "15 of CaCO 3 

. 56X-15 
therefore require 



.*. 56 x -15x70 . ,, 

00 - = grains of CaO per gallon. 

56 x -15x70x1000 

- - = grams of CaO per 1000 gallons, 

or 56 x -15 x 700 = 5880 grains ; 
there are 7000 grains per Ib. (16 oz.) - ^ QQQ 

= oz. per 1000 gallons ; or as one equation. 
56 x degrees of hardness x 16 

1000 

In actual calculations the percentage of CaO in the 
lime used must be known (140) and allowed for. 
Slaked lime is always used in practice ; the equation 
then becomes 

74 x degrees of hardness x 16 = oz. of Ca(OH) 2 

1000 
per 1000 gallons 

_ 74 x hardness x 16 x 100 
1000 x per cent, of Ca(OH) 2 in lime 
= oz. per 1000 gallons of slaked lime required. 

As the amount of C0 2 in the water always largely 

exceeds that required to keep the CaC0 3 in solu- 

tion, the above calculation will only give approxi- 

mately the amount of lime to be actually used. 

The following method of ascertaining the amount 



ANALYSIS OF FUEL, ETC. 83 

of lime (CaO) required per million parts of an 
ordinary water is taken from a paper by Mr. W. D. 
Collins in the Engineering Record, February 16, 
1907 (U.S.A.): 

(99) Excess o/C0 2 . Titrate 100 c.c. of the water 

with Na 2 C0 3 solution free from bicarbonate, 
ou 

using phenolphthalein as indicator. 

No. of c.c. used x 10 = CaC0 3 equivalent of 
CO 2 (a). 

(100) Temporary hardness. Titrate 100 c.c. of 

the water with H 2 S0 4 in a 200-c.c. graduated 
ou 

flask, using methyl orange as indicator. 

No. of c.c. used x 10 = parts per million of 
CaCO 3 (6). 

(101) Magnesia. Heat to boiling in the 200-c.c. 
flask the neutralised water (100); boil for fifteen 
minutes, add 25 c.c. of saturated lime water. Make 
up to 200 c.c. at temperature of room. Filter into 
a graduated cylinder, reject first 50 c.c., titrate next 

N 

100 c.c. with ^r H 2 S0 4 , using methyl orange as 
ou 

indicator. 

Repeat, using distilled water. 

Difference = amount of H 2 SO 4 which has been 
neutralised by Ca(OH) 2 required to ppt. MgO. 

This No. of c.c. x 20 = parts per million of CaC0 3 
equivalent to magnesia (c). 



84 CEMENT CHEMISTS 1 HANDBOOK 

(102) Permanent hardness. Boil 250 c.c. of the 

. N 
water in a porcelain dish. Add 25 c.c. of ^TT soda 

reagent (equal parts Na 2 CO 3 , NaOH), and boil for 
ten minutes. Filter, make up to 250 c.c., and titrate 

N 
100 c.c. with H 2 S0 4 . Repeat, using distilled 

water. Difference in number of c.c. of H 2 S0 4 re- 
quired = soda reagent used. 

This number x 10 = parts per million of CaCO 3 as 
permanent hardness (d). 



(103) Then a + b + cx '56 = parts per million of 
CaO required to soften water. 

d x 1*06 = parts per million of soda required to re- 
move permanent hardness. 

GAS ANALYSIS. Collection of Samples. 

A sample of rotary kiln or furnace gas can best 
be obtained at the base of the shaft. For this 
purpose a brass or copper tube sufficiently long 
is introduced through an eye-hole or an opening 
especially made. 

The length of tube inserted in the furnace should 
have holes pierced in the sides in order to obtain 
a sample of the gas from as many different points 
as possible. 

In order to prevent corrosion by acid gases, the 
tube may be dipped in a strong solution of borax 
and dried ; upon becoming heated the borax fuses 
and forms a protective glaze. Aspirators of metal 
or glass may be purchased, but for ordinary use a 



ANALYSIS OF FUEL, ETC. 85 

very effective one can be easily constructed from a 
Winchester quart bottle as follows : 

(104) Fit the bottle with a sound cork or rubber 
bung pierced with two holes. The cork is fitted 
with two glass tubes bent at right angles, one 
being sufficiently long to reach to the bottom of 
the bottle, the other only just passing through the 
cork. 

When the apparatus is to be used a glass or rubber 
tube sufficiently long to reach below the level of 
the bottom of the bottle is attached to the longer 
interior tube, the bottle is filled with water and 
suction applied to this tube ; the water is thus 
syphoned off, and the gas enters the other tube and 
fills the bottle. The rate of aspiration may be 
regulated by placing a screw clamp on the rubber 
connection. By preparing a number of bottles 
fitted in a similar way, but the glass tubes bearing 
glass stop-cocks, any number of samples of gas may 
be obtained with the use of one aspirator. 

(105) The apparatus is fitted up as fpllows 
Place the sampling tube in the flue ; to the end 
obtruding attach a wash bottle or a dust trap con- 
sisting of a tube loosely packed with asbestos or 
cotton wool ; connect this to the sample bottle and 
that in turn to the aspirator, making sure before- 
hand that all connections and stoppers are absolutely 
gas tight. Before sealing off and disconnecting the 
sample bottle, aspirate at least twice its volume of 
gas through the apparatus in order to remove air 



86 CEMENT CHEMISTS 1 HANDBOOK 

and to saturate the wash water with the gas under 
examination. 

Analysis of Gases in the Hempel Apparatus. In 
kiln or furnace gas it is necessary to estimate the 
following constituents when present : Carbon di- 
oxide, carbon monoxide, oxygen, nitrogen, and 
hydrocarbons. For a description of the apparatus, 
mode of fitting together, and other details Hempel's 
Gas Analysis should be consulted. 

The following solutions for absorption are re- 
quired : 

(106) For Carbon Dioxide. Dissolve 160 grams 
of KOH in 130 c.c. of distilled water. 

(107) For Oxygen. Dissolve 10 grams of pyro- 
gallol in 200 c.c. of potash solution (106). 

(108) For Carbon Monoxide. Dissolve a mixture 
of 86 grams of copper oxide (CuO) and 17 grams of 
copper filings in 1086 grams (969 c.c.) of hydro- 
chloric acid of sp. gr. 1'124, adding the mixture to 
the acid slowly with frequent stirring. Store in a 
bottle containing metallic copper. 

(109) Filling the Burette. Connect a piece of 
capillary glass tube to the top of the measuring 
tube of the burette by means of a piece of stout 
rubber tubing, which should carry a clip and be 
wired on. Fill the pressure tube with water satu- 
rated, if possible, with the gas under examination ; 
raise the tube, thus causing the water to enter the 
measuring tube until it issues from the capillary 



ANALYSIS OF FUEL, ETC. 87 

tube. Close the clip and connect to the aspirator 
by means of another piece of short rubber tube. 
All rubber connections should be wired on. Lower 
the pressure tube and open the clips until the gas to 
be analysed is drawn in and rather more than 100 
c.c. are contained in the measuring tube. 

Close the clips and disconnect from the aspirator, 
which must, of course, be again securely sealed up. 
Now close the long rubber tube between the pres- 
sure and measuring tubes. liaise the pressure tube 
and open the clip to allow water to flow into the 
measuring tube until it just reaches the graduation. 
Again close the clip on the connecting tube and 
open the top of the measuring tube ; excess of gas 
will escape, and exactly 100 c.c. will remain at 
atmospheric pressure ; close the clips. 

For technical work it is not necessary to note 
barometric pressure or temperature, provided they 
do not alter during the examination. 

(HO) Estimation of Carbon Dioxide. Fill an 
ordinary absorption burette with the potash solu- 
tion (106) by means of a funnel attached to the tube 
connected with the reservoir bulb. Then, by means 
of suction, draw the solution into the other (absorp- 
tion) bulb until it almost completely fills the capillary 
tube ; thus practically all air is excluded from the 
apparatus. Such an amount of reagent must be 
used that it will be contained by the reservoir bulb 
when it is driven back by the gas from the pipette. 
Having filled the burette, note the position of the 



88 CEMENT CHEMISTS 1 HANDBOOK 

reagent in the capillary tube and bring it to the 
same position between each reading. Attach the 
pipette by means of the connecting capillary tube 
and rubber joint. 

Open the pinch-cocks and raise the pressure tube, 
thus causing the gas to enter the burette. Allow 
the water to fill the connecting capillary tube, close 
the pinch-cocks, and gently shake the contents of the 
burette in order to present a larger surface of the 
reagent to the gas. Allow to stand for at least five 
minutes. Cause the gas to return to the pipette by 
lowering the pressure tube, adjust the level of the 
water, allow to stand for a few minutes, and then 
read off the volume of the gas. Repeat the operation 
until a constant volume is obtained. 

100 -- reading = volume of carbon dioxide per 
cent. 

Epitome. 

Treat 100 c.c. with potash solution in gas pipette. 

(111) Estimation of Oxygen. The pipette is re- 
placed by a " double" one containing alkaline pyro- 
gallate solution (107), and the absorption process 
repeated. 

Diminution in volume = oxygen per cent. 

(112) Estimation of Carbon Monoxide. The 
pipette is replaced by one containing acid cuprous 
chloride (108), and the absorption process repeated. 

Diminution in volume = carbon monoxide per 
cent. 



ANALYSIS OF FUEL, ETC. 89 

(113) Nitrogen. The residual gas is generally 
taken as consisting of nitrogen, and this is the case 
when the furnace is working properly. Should there 
be an insufficient supply of air, there may be hydro- 
carbons or hydrogen present. 

(114) Estimation of Combustible Gases. About 
30 c.c. of the residual gas are made up to 75 c.c. with 
oxygen, and the exact volume noted. The mixture 
is then fired in an explosion pipette or eudiometer 
by means of an electric spark. The contraction in 
volume is noted and the gas passed into the pipette 
containing potash solution (106), which absorbs the 
CO 2 formed, and the volume again noted. 

The volume of hydrogen and methane may be 
calculated as follows : 

Let x = contraction due to firing. 

y = after absorption of CO 2 . 

Vol. of hydrogen equals f (x Zy) 
methane equals y. 

The percentage is then calculated as follows : 

Vol. of hydrogen or methane x 

Vol. of residual gas 

. x 100 

Vol. taken for combustion 

(115) Analysis with the Orsat Apparatus. This 
is a portable apparatus consisting of a measuring 
burette and absorption pipettes, which are filled with 
the usual reagents. Some forms of the apparatus 
also have a palladium tube for the determination of 



90 CEMENT CHEMISTS 1 HANDBOOK 

the combustible gases. According to Hempel, there 
are several sources of inaccuracy. 

Full instructions are usually supplied with the 
instrument. It is a convenient apparatus for con- 
trol work. 

(ll6) To determine Conditions q/ Combustion in 
a Hotary Kiln. Let N = total per cent, of nitrogen 
found by analysis, and = total per cent, of oxygen 
found by analysis. 

The amount of nitrogen (N x ) corresponding to 
amount of air really useful in combustion is N a = 
nitrogen 376 oxygen. 

Without calculating the amount of air itself, we 
can obtain a ratio between the air introduced and 
the air used, thus : 

100 N 
N^- 376 oxygen 

gives a value either more or less than 100. If a 
ratio above 100 is found, it shows that excess of air 
is being used, and vice versd, in which case com- 
bustible and reducing gases will be found. In a 
rotary kiln there should always be a slight excess of 
oxygen to prevent the formation of ferrous com- 
pounds in the clinker. 

The above calculations are from vol. iii. Geo. 
Survey Ohio, by Professor Orton. 



CHAPTER V 
CEMENT ANALYSIS 

(117) Accurate Methods. Weigh out into a 
6-in. flat porcelain or platinum dish 0'5 gram of the 
cement. Add a little distilled water, and rotate 
the dish to prevent setting; then add 25 c.c. of 
pure 10E HC1, place on a sand or water bath, and 
evaporate to dryness. Cover with a clock glass, and 
bake on a hot plate at a temperature of 200 C. for 
at least one hour. Remove from hot plate, and 
allow to cool. Add 25 c.c. of 10E HC1 and about 
the same amount of water, warm for a few minutes 
on the sand or water bath until the insoluble matter 
is quite free from iron compounds. Filter through 
a 12'5-cm. black band filter paper, wash by decanta- 
tion, remove every trace of silica adhering to the 
dish by means of a rubber- tipped glass rod. Wash 
with hot water until quite free from chloride. Re- 
turn the filtrate to the dish, and again evaporate to 
dryness on the sand bath. 

Take up with 25 c.c. 10E HC1 and water, digest 
if necessary, filter off any trace of silica through a 
9 -cm. paper, and wash well. Dry and ignite the 

91 



92 CEMENT CHEMISTS 1 HANDBOOK 

two residues together for at least one hour in a good 
muffle furnace. 

Weight ash of filters x 200 = silica + insolu- 
ble. 

(118) Alumina and Ferric Oxide. Eeturn 
the filtrate from (117) to the evaporating dish, add 
a drop or two of bromine water, and bring nearly 
to the boiling-point over an argand burner or on 
a hot plate. Cautiously add a slight excess of 
10E NH 4 OH, and gently heat until nearly all the 
excess of ammonia has been driven off. Filter 
through a 15-cm. black band paper, using a "cut 
funnel " ; wash slightly, and collect the filtrate in a 
large Phillips beaker. Pierce a hole in the filter 
paper and wash the ppt. back into the original 
dish. Without removing paper from the funnel, 
drop on to it 15 c.c. of 10E HC1, and wash down 
into the dish with about 20 c.c. of hot water. Re- 
precipitate the alumina and iron oxide as before, 
filter, and wash thoroughly and rapidly, well churn- 
ing up the ppt. Dry, and ignite in muffle for one 
hour, cool in desiccator and weigh. 

Weight -- ash of filter x 200 = per cent, of 
A1 2 O 3 + Fe 2 3 . 

(119) Lime (CaO). Evaporate the filtrate (118) 
somewhat, if necessary, and heat nearly to boiling ; 
add about 20 c.c. of 5E NH 4 OH, boil and add at 

TT 

least 30 c.c. of boiling ammonium oxalate solution, 

o 

and continue to boil for five minutes. Allow to 



CEMENT ANALYSIS 93 

stand in a warm place, if possible, for at least one 
hour. Filter through a Swedish or white band 
15-cm. paper and wash. The filtrate and first 
washings are reserved for MgO determination (121). 
Continue the washings until a drop of the filtrate 
does not discolour an acidified very dilute solution 
of potassium permanganate. Estimate CaO by 
means of standard solution of permanganate, as 
described in (9) ; or as CaSO 4 (10). 

(120) For very accurate work ignite the wet.ppt. 
in a platinum crucible over a small bunsen burner. 
Place in a large beaker, dissolve ppt. in redistilled 
10E HC1, dilute with 150 c.c. of water, warm, add 
slight excess of 10E NH 4 OH, filter off any traces 
of alumina, reprecipitate with ammonium oxalate, 
and estimate the CaO as before, or ignite in good 
muffle to constant weight. 

Weight of CaO - filter ash x 200 = per cent. CaO. 

(121) Magnesia (MgO). The filtrate or filtrates 
from (119) are evaporated nearly to dry ness in the 
large dish. Add 30 c.c. of pure 16E HNO 3 , evapo- 
rate to dry ness, and continue heating on the hot plate 
until all ammonium salts are volatilised. Remove 
from plate and dissolve residue in 5 c.c. of 10E HC1 
and about 20 c.c. of distilled water. Add one drop 
of bromine water and slight excess of 10E NH 4 OH, 
boil carefully for a few minutes and then filter off 
any ppt. through a 5 -cm. black band paper. If not 
exceeding 0'002 gram, ignore. Collect filtrate in 
a 200-c.c. beaker, add 10 c.c. of 20E NH 4 OH and 



94 CEMENT CHEMISTS 1 HANDBOOK 

2E 
5 c.c. of -^- Na 2 HPO 4 solution. Stir well with a 

o 

rubber-tipped rod, and allow to stand in a cool 
place over night. 

Filter through a 7 or 9 cm. filter paper, wash by 
decantation, using 5E NH 4 OH ; then transfer ppt. 
to the paper, remove by means of the rubber-tipped 
glass rod any particles adhering to the sides of the 
beaker, and continue to wash until free from 
chlorides. The ppt. may be ignited while moist in 
a platinum or porcelain crucible in the muffle furnace 
or over a good burner for half an hour. Cool in a 
desiccator and weigh as Mg 2 P 2 O 7 . 

40 
Weight of ppt. x r T x 20() =per cent, of MgO 

(see Appendix, 25A). The ppt. before washing may be 
dissolved in a little warm water and a drop of hydro- 
chloric acid, and repptd. by addition of 1 c.c. of 

o"P 

-- Na 2 HPO 4 and excess of ammonia. 



(122) Alkalies. These are generally estimated 
by difference ; they may be estimated directly by 
the Lawrence Smith method as described under Clay 
(31), or as follows. 

Treat one gram of cement in a large platinum 
dish, as for ordinary analysis for estimation of Si0 2 , 
R 2 O 3 , CaO. Evaporate filtrate from CaO deter- 
mination to dryness in a platinum dish carefully. 
Ignite residue until free from ammoniacal salts, cool, 
then add 5 c.c. of water and brush in about 1 gram 



CEMENT ANALYSIS 95 

of powdered oxalic acid crystals. Evaporate care- 
fully to dryness and ignite as before. Treat the 
residue with about 20 c.c. of hot distilled water, 
filter, and wash ; residue consists of MgO and may 
be weighed as such. 

The filtrate is made acid with 10E HC1 and 
evaporated to dryness very carefully in a weighed 
platinum dish. Cool in a desiccator and weigh. 

Weight = NaCl + KCl. 
Na 2 O and K 2 O can then be estimated as under 31 A. 

Epitome. 

Separate Si0 2 , A1 2 O 3 , Fe 2 3 , CaO. 

Evaporate to dryness, add oxalic acid and water, 
evaporate to dryness, take up with water, filter and 
wash. Acidify filtrate with hydrochloric acid and 
evaporate. 

Separate KC1 and NaCl by means of platinum 
chloride (see 31 A). 

(123) Ordinary Method of Analysis for 
Technical Purposes. Si0 2 and insoluble. 
Weigh out 0*5 gram of cement into a 6 -inch porcelain 
dish, add a little water, swirl round, and add 25 c.c. 
10E HC1. Evaporate to dryness on hot plate, cover, 
and bake for one hour. Remove from hot plate, 
and when nearly cool take up with 25 c.c. 10E HC1 
and water. Digest, if necessary ; filter off Si0 2 + 
insoluble, clean dish, well wash, ignite and weigh. 

Weight x 200 = per cent, silica and insoluble. 



96 CEMENT CHEMISTS 1 HANDBOOK 

(124) AI Z 39 Fe 2 O 3 .To filtrate from (123) con- 
tained in the large dish add a drop or two of 
bromine water and slight excess of 10E NH 4 OH ; 
gently boil off excess of ammonia, filter through a 
black band rapid paper, wash well, ignite and weigh 

Weight x 200 = per cent. A1 2 3 , Fe 2 O 3 . 

(125) CaO.Boil filtrate from (124) in a large 
Phillips beaker, add slight excess of ammonia and 

^T? 

50 c.c. of boiling ammonium oxalate, boil for 
o 

three minutes, allow to stand for half an hour, filter, 
wash well, and estimate by means of standard 
permanganate (9). 

(126) Evaporate filtrate from (125) nearly to 
dryness, add 30 c.c. of 16E HN0 3 and drive off 
ammonium compounds. Take up with a few drops 
of hydrochloric acid and a little water. Add 
slight excess of ammonia, filter off any ppt., to 

9TT 

filtrate add 10 c.c. 10E NH 4 OH and 5 c.c. of 

3 

Na 2 HPO 4 , stir well or shake in a stoppered bottle 
vigorously, allow to settle, filter, wash with 5E 
NH 4 OH, and weigh as Mg 2 P 2 O 7 (25A). 

40 
Weight x x 200 = per cent. MgO. 

Epitome. 

Treat 0'5 gram cement with 25 c.c. hydro- 
chloric acid, and evaporate to dryness. Bake 
one hour, allow to cool, take up with 25 c.c. 



CEMENT ANALYSIS 97 

hydrochloric acid. Filter, wash, ignite, and 
weigh = SiO 2 4- insoluble. Ppt. A1 2 O 3 , Fe 2 O 3 
with ammonia. Filter, wash, ignite, and 
weigh = A1 2 O 3 , Fe 2 O 3 . To filtrate add 
boiling ammonium oxalate + ammonia. 
Filter, wash, estimate = CaO. Evaporate 
filtrate nearly to dryness, add 30 c.c. nitric 
acid, drive off all Am. salts. Dissolve in dilute 
hydrochloric acid, ppt. and filter off traces of 
Al 2 O 3 ,Fe 2 O 3 ; ignore ppt. To filtrate add 
ammonia + sodium phosphate, agitate, allow 
to settle, filter, wash with 5E NH 4 OH, ignite 
and weigh as Mg 2 P 2 O 7 ; calculate to MgO. 

(127) Insoluble Residue. Weigh out into a 
5 -in. flat porcelain dish 0*5 gram of cement. Add a 
little distilled water and rotate to prevent setting ; 
then add 10 c.c. of 10E HC1 and place on the hot 
plate for ten minutes or a quarter of an hour. It is 
not essential that the contents of the dish should be 
evaporated to dryness, but it is preferable to do so, 
if time permits. 

Add, in either case, 10 c.c. of 10E HC1 and about 
25 c.c. of water, allow insoluble matter to settle, 
filter through a 9-cm. black band paper, wash at 
least three times by decantation, allowing as little of 
the insoluble matter as possible to leave the dish. 
Finally, wash back into the dish any particles 
adhering to the filter paper without removing latter 
from the funnel. The filtrate is used for estimation 
of SO 3 (128). To the contents of the dish add 



98 CEMENT CHEMISTS 1 HANDBOOK 

10 c.c. of 3E Na 2 G0 3 solution and boil for ten 
minutes. Filter rapidly through the paper pre- 
viously used, and wash with boiling water until a 
drop of the filtrate leaves no residue upon evapora- 
tion. Dry, ignite, and weigh. 

Weight - filter ash x 200 = per cent, insoluble 
residue. 

The weight so obtained is subtracted from the 
total Si0 2 and insoluble residue (123). 

Epitome. 

Treat 0*5 gram with warm hydrochloric acid. 

Filter, wash by decantation. 

Boil residue with 10 c.c. sodium carbonate 

solution. 
Filter, wash, ignite, and weigh. 

(128) Sulphuric Anhydride (SO 3 ). Boil in a 
10-oz. Phillips beaker the filtrate from (127), and 
whilst still boiling add drop by drop 10 c.c. of 
E BaCl 2 solution ; after five minutes allow to 
settle in a warm place for at least two hours, if 
possible. Filter through a 7-cm. No. 417A Max 
Dreverhoff paper, wash with warm water until quite 
free from chloride. Dry, ignite, and weigh as 
BaS0 4 . The damp paper may be placed in the 
mouth of the muffle furnace and ignited therein 
afterwards with out much fear of an inaccurate 
result. 

on 

Weight of BaS0 4 x * 200 = per cent. S0 3 . 



CEMENT ANALYSIS 99 

Epitome, 

Precipitate with barium chloride solution. 
Wash, ignite, and weigh as BaSO 4 . 

(129) Sulphur as Sulphide. Sulphides, if 
present in sufficient amount, may be estimated by 
the following method. Treat 0'5 or 1 gram of 
cement with a little water in the usual way, then 
add 25 c.c. of 16E HNO 3 , warm and evaporate 
gently to dryness, allow to cool, and take up with 
10 c.c. of 10E HC1 and water. Filter off silica and 
wash. 

To the filtrate add 10 c.c. of E BaCl 2 solution and 
treat as in (128). From the weight of BaSO 4 
obtained deduct the equi\ r alent found when esti- 
mating SO 3 . The excess BaSO 4 x 0'137 x 200 (or 
100) = per cent, sulphur as sulphide. 

Epitome. 

Treat with nitric acid, evaporate, take up with 
hydrochloric acid, filter and wash. 

To filtrate add BaCl. 2 solution, filter, wash, weigh 
as BaSO 4 . 

The sulphur found as sulphide may be calculated 
to calcium sulphide, CaS, thus : 

Weight of BaS0 4 x 0-30895 x 200 - CaS, 
in which case the equivalent must be deducted from 
the lime (CaO) found. One per cent, of CaS = 0'78 
per cent. CaO. In like manner S0 3 may be con- 
verted into CaS0 4 . 



100 CEMENT CHEMISTS' HANDBOOK 

Weight of BaSO 4 x *|| x 200 = CaSO 4 . 

For each 1 per cent, of CaSO 4 deduct 0'41 per cent, 
from the CaO found. 

(130) Loss on Ignition. 0'5 gram is ignited in 
a platinum capsule for ten minutes in a muffle 
furnace. The temperature should not exceed 800 C., 
or there will be a loss of S0 3 . 

Loss in weight x 200 = loss on ignition (CO 2 + H 2 0). 

Carbon Dioxide. If necessary this may be 
estimated by treating 5 grams with hydrochloric 
acid in the absorption apparatus as described in (14). 

(131) R. K. Meade (Portland Cement) recom- 
mends the use of a Shinier crucible. This consists 
of a platinum crucible provided with a water- 
jacketed stopper and reservoir for supplying water 
to the latter. From 1 to 3 grams of cement are placed 
in the crucible and covered with ignited asbestos. 
The crucible is heated by means of a bunsen burner 
after starting a flow of hot water through the stopper. 
The gas is aspirated through potash bulbs and 
calcium chloride tubes in the usual way. Finally 
the crucible is heated over a blast burner. The 
absorption apparatus is weighed ; increase of weight 
equals C0 2 . If the cement contains any unburnt 
carbonaceous material this causes an error. The 
carbon may be estimated by treating the cement 
with acid, filtering through asbestos, and then 
igniting residue in the crucible. For details see 
work cited. 



CEMENT ANALYSIS 

(132) Rapid Method for Estimation of Lime 
in a Cement. Weigh 0'5 gram of cement into a 
dry wide-form 800-c.c. beaker, add about 10 c.c. of 
distilled water, and rotate to prevent setting, then 
add 20 c.c. of 10E HC1. Warm until solution is com- 
plete. Dilute to about 250 c.c. with warm water, 
boil for a few minutes, then exactly neutralise with 
10E NH 4 OH, using methyl orange as indicator. To 

^TT 
the boiling solution add 10 c.c. of (concentrated) 

oxalic acid solution, boil for one minute, then add 

3E 

70 c.c. of ammonium oxalate solution. Boil 
5 

for seven minutes, remove from heat, allow to settle, 
and filter through a 15 -cm. black band paper. 
Wash several times by decantation, using plenty of 
hot water ; then transfer to filter paper and wash 
until a drop of the filtrate acidified with sulphuric 
acid will not decolourise water faintly tinged with 
permanganate. About 700 c.c. of wash water will 
be required ; with practice, always using the same 
quantity of reagents, one can readily gauge the 
amount of warm water to use. 

Remove the filter from the funnel, open and lay 
against the sides of the beaker in which precipitation 
was made. Wash ppt. from the paper into the 
beaker. Add 30 c.c. or sufficient 5E H 2 S0 4 , warm, 
titrate with standard permanganate, of which the 
strength in terms of CaO is known. 

No. of c.c. used x factor x 200 = CaO. 



102 CEMENt CHEMISTS' HANDBOOK 

(133) The permanganate is best standardised 
against pure Iceland spar, taking a known weight of 
spar and following through the process described 
(132). A convenient strength is obtained by using 
6-7 grams of permanganate per litre. 

(134) ANALYSIS OF GYPSUM, PLAS- 
TER, KEENE'S CEMENT, Etc. All these 
bodies consist of calcium sulphate in one form or 
another. The necessary estimations include silica + 
insoluble matter, alumina and iron oxide, lime, mag- 
nesia, sulphuric anhydride, and water. 

(135) Silica and Insoluble. Weigh out into 
a porcelain or platinum dish 1 gram of the finely 
powdered material. Add a little water and rotate 
to prevent setting. Add 10 c.c. 10E HC1 and 
evaporate carefully to dryness. Take up with 25 c.c. 
of 10E HC1 and water. Digest, if necessary ; filter 
off through a small filter paper any insoluble matter, 
wash well, dry, ignite, and weigh. 

Weight filter ash x 100 = per cent, insoluble. 

(136) Make the filtrate up to 500 c.c. and divide 
into two parts of 250 c.c. each. 

Alumina + Ferric Oxide, Lime, and Mag- 
nesia. In one portion estimate A1 2 O 3 , Fe 2 O 3 , CaO, 
and MgO by the ordinary methods. 

(137) Sulphuric Anhydride. Place the other 
portion of 250 c.c. in a fairly large beaker and bring 
to the boil ; whilst gently boiling, add 20 c.c. of 



CEMENT ANALYSIS 103 

E BaCl 2 drop by drop. Allow ppt. to settle, filter, 
wash, ignite, and weigh. 
Weight - filter ash x '34291 x 200 = per cent. S0 3 . 

This may be converted into CaSO 4 as shown under 
(129). 

(138) Water. Ignite 0*5 gram in a platinum 
crucible in the muffle at a temperature of about 
400 C. for twenty minutes. Care must be taken to 
avoid loss of SO 3 or reduction to sulphide. 

Loss in weight x 200 = per cent. H 2 0. 

(139) ESTIMATION OF CAUSTIC 
LIME (CaO) IN BURNT LIME. The 

material under examination should be sampled, 
crushed, and finely powdered as rapidly as possible. 
The original sample should be stored in an air-tight 
receptacle, and the portion for analysis placed in a 
dry weighing tube. 

(140) Estimation of CaO. Transfer about 0*5 
gram of the finely powdered sample into an Erlen- 
meyer flask containing about 250 c.c. of air-free dis- 
tilled water. Boil gently for five minutes, close tne 
flask with a cork bearing a soda-lime tube, and allow 

N 
to cool. When quite cold, titrate with -~~ HC1, 

using phenolphthalein as indicator ; allow the flask 
to remain some time to see if the pink colouration 
returns. 

No. of c.c. used x '0028 x 100 

weight taken " = P er cent ' Ga - 



APPENDIX 



APPENDIX 



EXAMPLES OF CALCULATIONS 
OCCURRING DURING ANALYSIS 



171 



(!A) Clay Analysis. Conversion of insoluble 
into felspar (21). 

Found. Insol. 12 '8 8 per cent, containing 
per cent. R 2 O 3 " 

then 171 x 3'5 = 5 '98 per cent. SiO 2 
171 x 0-6 = 1-02 



Na 2 



+ TiO 2 found 
+ R 2 O 3 ,, 



24 
171 
8-95 



12*88 -- 8-95 = 3-93 percent, of quartz. 

Report as follows : 

SiO 2 =5-98 

-felspar 



Insoluble matter 12 '8 8 



A1 2 3 
Na 2 O 
TiOo 



= 5-98 
= 171 
= 1-02. 
= -24 



Quartz =3'93 
12-88 

(2A) To ascertain proportions of limestone and 
sbale to obtain desired mixture. 

107 



108 CEMENT CHEMISTS' HANDBOOK 

Ultimate Analysis. 

Limestone. Shale, 

SiO 2 = 5'96 4974 

A1 2 O 3 = 2-00 15*98 

Fe 2 3 = 0-90 8-00 

CaO =49-38 9-08 

MgO = 1-12 4-03 

Loss on ignition =40'12 10'04 

Alkalies and loss = 0'52 3*13 

100-00 100-00 

Calculation. 
Limestone. 

SiO 2 = 5-96x2-8 =16'688 
ALOo = 2'OOx 1-1 = 2-200 



18-888* 
Shale. 

Si0 2 = 49-74 x 2-8 = 139'272 
A1 2 3 = 15-98x1-1 = 17-578 

157-850 

CaO = 49-380 157'85 

-18-888* -CaO in shale 9'08 



y =30-492 a =14877 

14877x100 
Then 30-492 =487>9 

Therefore 100 parts of shale should require 487'9 
parts of limestone, or 

Limestone 4 '8 parts 
Shale ro part 



APPENDIX 109 

(3 A) To produce mixture containing 75 per cent. 
CaCO 3 ; same materials. 

CaCO 3 in limestone = 88*1 8 per cent. 
Per cent, required =75*00 ,, 

Shale required =13*18 parts. 

- - f 

Per cent, required =75*00 

CaCO 3 in shale =16*21 
Limestone required = 58*79 parts. 

or Limestone 4*4 parts. 
Shale 1*0 part 

(4A) Analysis of Slurry (54). 

Example of calculation : 

CaC0 3 = 75*2 per cent. = CO 2 33*08 per cent, (B). 
Loss on ignition = 33*80 per cent. (A). 

Then 33*80 
-33*08 



= 0*72 loss due to organic matter (C). 
and 100 -- 0*72 = 99*28 (D). 



= 75*74 calculated CaCO 3 . 



(5 A) Calculated CaO (55). 
Lime in residue after ignition = 42*4 per cent. 
Loss on ignition =33*8 

1QQ oo. 8 = 64 per cent, calculated CaO in clinker. 



110 CEMENT CHEMISTS 1 HANDBOOK 

(GA) Directions for making up E Solutions. 

Hydrochloric acid (sp. gr. 1-16) = 10E HC1. 
( 1-08) = 5E HC1. 
200 c.c. of 5E HC1 

diluted to 1 litre = E HCl 
Nitric acid (sp. gr. 1-5) -24E HN0 3 . 

( 1-42) = 5EHN0 3 . 

Sulphuric acid (sp. gr. 1-842) = 36E H^SO^ 

Acetic acid (glacial) = 17E Ac. 

294 c.c. 17E diluted to 

1 litre = 5E Ac". 

Oxalic acid 9 4 '5 grams dissolved 

and diluted to make 

3 

1 litre =2 Eox ' 

Ammonium hydrate ('880) = 20E NH 4 OH 

equal volumes 

of 20E and 

distilled water = 10E NH 4 OH 
oxalate 42*6 grams dis- 

solved and diluted 

o 

to 1 litre = ^.E Am. ox. 

carbonate 1967 grains 

dissolved in 333*3 c.c. 
of 5E NH 4 OH and 
diluted to 1 litre = 5E Am 2 C0 3 
Sodium hydrate 200 grams dis- 
solved to make 1 litre = 5E NaOH 
,, carbonate 429 grams of 

crystals to make 1 litre = 3E Na 2 C0 3 



APPENDIX 111 

Sodium hydrogen phosphate 119*3 
grams of crystals dis- 
solved to make 1 litre = E Na 2 HPO 4 

o 

sulphite 252 grams of 

crystals to make 1 litre = 4E Na 2 SO 3 
acetate 544 grams of 

crystals to make 1 litre = 4E Na Ac. 

Potassium hydrate 280 grams to 

make 1 litre = 5E KOH 

iodide 166 grams to 

make 1 litre =E KI 

chromate 97*25 grams 

to make 1 litre = E K 2 Cr0 4 
ferrocyanide 105*5 

grams to make 1 litre = E K 4 FeC 6 N 6 
,, ferri cyanide 109*7 

grams to make 1 litre = E K 3 FeC 6 N 6 
, , sul phocy anide 9 7 grams 

to make 1 litre = E KCNS 

Bromine water water at 15*5 C. 

pi 

saturated with Br = Br water 

2i 

Barium chloride 122 grams dis- 
solved to make 1 litre = E Ba'Cl 2 

Silver nitrate 170 grams dissolved 

to make 1 litre = E AgNO 3 
34 grams dissolved 

Tjl 

to make 1 litre = ,, 



112 CEMENT CHEMISTS' HANDBOOK 

Mercuric chloride 24 '2 grams dis- 

2E 

solved to make 1 litre = ^- HgCL 

o 

Copper sulphate 12475 grams of 

crystals to make 1 litre = E CuSO 4 

Platinic chloride 49*3 grams of Pt 
converted into PtCl 4 and di- 
luted to 1 litre = E PtCl 4 

Magnesia mixture 68 grams 
MgCl 2 6H 2 O in about 500 c.c. 
H 2 O, add 165 grams AmCl, 
300 c.c. 5E NH 4 OH and dilute 
to 1 litre = E Mg Mixt. 

Ammonium molybdate. Dissolve 90 grams in 700 
c.c. of water, allow to settle and decant ; dilute 
to 1 litre. 

Fusion mixture 

106 grams of dry Na 2 C0 3 
138 " K 2 C0 3 
well mixed and ground together. 

Mixture for Hundeshagen's method (63) for sulphur 
in fuels 

MgO 2 parts by weight 
K 2 C0 3 1 part 
dried and ground together. 

Copper sulphate pumice for absorption (14) of HC1 + 

H 2 0- 

Soak some pieces of pumice stone free from dust 
in a saturated solution of CuS0 4 . When 



APPENDIX 113 

thoroughly saturated, dry and ignite until free 
from blue colour. Store in a well-stoppered 
bottle. 



PREPARATION OF STANDARD 
SOLUTIONS 

(7A) Normal Sodium Carbonate, N.Na 2 C0 3 . 
Dissolve exactly 53 grams of Na 2 C0 3 (prepared 
by igniting bicarbonate) in distilled water and make 
up to 1000 c.c. 

1 c.c. = '053 gram Na. 2 CO 3 
= '022 C0 2 

N 
(8A) Deci-normal Na 2 CO 3 = ^ Na 2 CO 3 . 

Dissolve 5*3 grams in 1000 cc. of distilled water. 

1 c.c. = -0053 gram Na 2 CO 3 . 
(9A) Normal Sulphuric Acid, N.H 2 SO 4 . 
Dilute about 30 c.c. of cone. H 2 SO 4 (sp. gr. 1-840) 
to 1 litre. Add the acid to less than 1000 c.c. of 
water, and, when cool, titrate against N.Na 2 C0 3 , 
using methyl orange as indicator. Then measure 
the solution and dilute to correct bulk. 
1 c.c. = -049 gram H 2 SO 4 . 

N 
(lOA) Deci-normal Sulphuric Acid, TT; H 2 SO 4 . 

Dilute 100 c.c. of normal H 2 SO 4 to 1000 c.c. and 

N 
standardise against r^ Na 2 CO 3 . 

1 c.c. = -0049 gram H 2 SO 4 . 



114 CEMENT CHEMISTS' HANDBOOK 

(HA) Normal Hydrochloric Acid, N.HC1. 

Dilute 150 c.c. of pure HC1 (sp. gr. 1-16) to 1000 
c.c., titrate with N.Na 2 CO 3 and correct accordingly. 
1 c.c. = '0365 gram HC1. 

N 
(12A) Deci-normal HOI, y^ HOL 

Dilute 100 c.c. of N. HC1 to 1000 c.c. with distilled 
water. 

1 c.c. = '00365 gram HC1. 

(13A) Normal Sodium Hydrate, N. NaOH. 

Dissolve about 44 grams of stick NaOH, free from 
carbonate, in about 1000 c.c. of distilled water. 
Titrate, when cool, against normal H 2 SO 4 and dilute 
accordingly ; use methyl orange or phenolphthalein 
as indicator. 

1 c.c. = '040 gram NaOH. 

(14A) Deci-normal NaOH. 

Dilute 100 c.c. N. NaOH to 1000 c.c. with distilled 
water. 

1 c.c. = '0040 gram NaOH. 

(15 A) Normal Potassium Hydrate, N. KOH. 

Dissolve 56 grams in less than 1000 c.c. of water, 
titrate against N. H 2 S0 4 , and dilute accordingly. 
For alcoholic KOH use 90 per cent, alcohol. 
1 c.c. = -056 gram KOH. 

(16A) Deci-normal KOH, ^ KOH. 

Dilute 100 c.c. of normal KOH to 1000 c.c. and 
standardise. 

1 c.c. = -0056 gram KOH. 



APPENDIX lis 

(I?A) Deci-normal Potassium Permanga- 

N 
nate, ^ K 2 Mn 2 8 . 

Dissolve 3*156 grams of potassium permanganate 
in distilled water and dilute to 1000 c.c. Titrate 
with pure iron wire, ferrous ammonium sulphate, or 
oxalic acid. 

N 
1 c.c. r^ K 2 Mn 2 O 8 = -0056 gram Fe. 

= -0072 FeO. 
= -0080 Fe 2 O 3 . 

(ISA) Deci-normal Potassium Bichromate, 
^ K 2 Cr 2 7 . 

Dissolve 4 '9 13 grams of fused crystals in water 
and make up to 1000 c.c. 

1 c.c. = -0056 gram Fe. 

This solution requires standardisation after a time. 
Use potassium ferricyanide on a spotting tile as 
indicator. 

N 
Deci-normal Silver Nitrate, AgNO 3 . 

Dissolve 16*998 grams in distilled water and make 
up to 1000 c.c. 

1 c.c. = -003545 gram 01. 



116 



CEMENT CHEMISTS 1 HANDBOOK 



INDICATORS. 

(19 A) Litmus Solution. Digest the solid with dis- 
tilled water for several hours. Decant or filter, 
render neutral by means of acetic acid or ammonia. 
Store in a bottle with access of air. 

(20A) Methyl Orange. Dissolve about 1 gram of 
the solid in distilled water and make up to 1 000 c.c. 

(21 A) Phenolphthalein. Dissolve a little of the 
solid in alcohol and dilute with alcohol and water. 



(22A) TABLE OF ATOMIC WEIGHTS OF PRIN- 
CIPAL ELEMENTS OCCURRING IN CEMENT 
WORKS ANALYSIS. 



Aluminium 


Al 


27-11 


Nitrogen 


N 


14-01 


Barium 


Ba 


137-43 


Oxygen 


O 


16-00 


Calcium 


Ca 


40-10 


Phosphorus 


P 


31-00 


Carbon 


C 


12-00 


Platinum 


Pt 


194-80 


Chlorine 


Cl 


35-45 


Potassium 


K 


39-15 


Copper 


Cu 


63-60 


Silicon 


Si 


28-40 


Hydrogen 


H 


1-008 


Silver 


Ag 


107-93 


Iron 


Fe 


55-90 


Sodium 


Na 


23-05 


Magnesium 


Mg 


24-36 


Sulphur 


S 


32-07 


Manganese 


Mn 


55-00 


Titanium 


Ti 


48-10 



APPENDIX 117 



(23A) FACTORS FOR USE IN ANALYSIS, 

Kequired. Known. Factor. 

CaO CaC0 3 0*56043 

CaC0 3 CaO 1-78431 

C I C0 2 0-27272 

Fe Fe 2 3 0-69953 

Fe 2 3 Fe 1*42933 

H 2 S0 4 BaS0 4 0-42007 

S 0-13734 

S0 3 0-34291 

K 2 O K 2 PtCl 6 0-19411 

K 2 O KC1 0-63204 

Na 2 NaCl 0'53077 

MgO Mg 2 P 2 7 0-36242 

P 0*63757 



118 



CEMENT CHEMISTS 1 HANDBOOK 



(24A) LIME IN CEMENT (119). 



Milligrams 
of 
CaSO 4 . 


Per cent. 
CaO. 


Milligrams 
of 
CaSO 4 . 


Per cent. 
CaO. 


Milligrams 
of 
CaSO4. 


Per cent. 
CaO. 


690 


56-82 


720 


59-28 


750 


61-75 


691 


56-90 


721 


59-36 


751 


61-83 


692 


56-98 


722 


59-45 


752 


61-91 


693 


57-08 


723 


59-53 


753 


62-00 


694 


57-16 


724 


59-61 


754 


62-08 


695 


57-23 


725 


59-70 


755 


62-16 


696 


57-32 


726 


59-79 


756 


62-24 


697 


57-40 


727 


59-86 


757 


62-32 


698 


57-48 


728 


59-94 


758 


62-41 


699 


57-56 


729 


60-02 


759 


62-49 


700 


57-63 


730 


60-10 


760 


62-57 


701 


57-72 


731 


60-19 


761 


62-65 


702 


57-80 


732 


60-27 


762 


62-74 


703 


57'88 


733 


60-35 


763 


62-82 


704 


57-97 


734 


60-43 


764 


62-90 


705 


58-06 


735 


60-51 


765 


62-99 


706 


58-14 


736 


60-60 


766 


63-07 


707 


58-22 


737 


60-68 


767 


63-15 


708 


58-30 


738 


60-76 


768 


63-23 


709 


58-38 


739 


60-85 


769 


63-31 


710 


58-46 


740 


60-93 


770 


63-40 


711 


58-54 


741 


61-01 


771 


63-48 


712 


58-62 


742 


61-09 


772 


63-56 


713 


58-70 


743 


61-18 


773 


63-64 


714 


58-79 


744 


61-26 


774 


63-72 


715 


58-87 


745 


61-34 


775 


63-81 


716 


58-96 


746 


61-42 


776 


63-89 


717 


59-04 


747 


61-50 


777 


63-98 


718 


59-12 


748 


61-59 


778 


64-06 


719 


59-20 


749 


61-67 


779 


64-14 



APPENDIX 



119 



(25A) TABLE FOR ESTIMATION OF MgO IN 
CEMENT (126). 

MAGNESIA, USING '5 GRAM OF CEMENT. 



Weight of 
Mg 2 P 2 7 . 


MgO 
per cent. 


Weight of 

Mg 2 l* 2 O 7 . 


MgO 
per cent. 


Weight of 
Mg 2 l> 2 7 . 


MgO 
per cent. 


Gram. 




Gr;im. 




Gram. 




0080 


0-57 


0195 


1-41 


0310 


2-23 


0085 


0-61 


0200 


1-44 


0315 


2-26 


0090 


0-65 


0205 


1-48 


0320 


2-30 


0095 


0-68 


0210 


1-51 


0325 


2-33 


0100 


0-72 


0215 


1-55 


0330 


2-37 


0105 


0-76 


0220 


1-58 


0335 


2-40 


0110 


0-79 


0225 


1-62 


0340 


2-44 


0115 


0-83 


0230 


1-66 


0345 


2-48 


0120 


0'86 


0235 


1-69 


0350 


2-52 


0125 


0-90 


0240 


1-73 


0355 


2-55 


0130 


0-94 


0245 


1-76 


0360 


2-59 


0135 


0-97 


0250 


1-80 


0365 


2-62 


0140 


1-01 


0255 


1-83 


0370 


2-66 


0145 


1-04 


0260 


1-87 


0375 


2-70 


0150 


1-08 


0265 


1-91 


0380 


2-74 


0155 


1-12 


0270 


1-94 


0385 


2-77 


0160 


1-15 


0275 


1-98 


0390 


2-80 


0165 


1-19 


0280 


2-01 


0395 


2-84 


0170 


1-23 


0285 


2-05 


0400 


2-88 


0175 


1-26 


0290 


2-08 


0405 


2-92 


0180 


1-30 


0295 


2-12 


0410 


2-95 


0185 


1-33 


0300 


2-15 


0415 


2-98 


0190 


1-37 


0305 


2-19 


0420 


3-02 



CEMENT CHEMISTS 1 HANDBOOK 



(26A) TABLE FOR ESTIMATION OF SO 3 IN 
CEMENT (128). 

SO,, USING -5 GKAM OF CEMENT. 



Weight of 
BaS0 4 . 


SO 3 per 
cent. 


CaSO 4 per 
cent. 


Weight of 
BuS0 4 . 


SO 3 per 
cent. 


CaSO 4 per 
cent. 


0100 


0-68 


1-16 


0205 


1-41 


2-39 


0105 


0-71 


1-22 


0210 


1-44 


2-45 


0110 


0-75 


1-28 


0215 


1-48 


2-51 


0115 


0-79 


1-34 


0220 


1-51 


2-57 


0120 


0-82 


1-40 


0225 


1-55 


2-63 


0125 


0-86 


1-46 


0230 


1-58 


2-68 


0130 


0-89 


1-52 


0235 


1-61 


2-74 


0135 


0-92 


1-57 


0240 


1-65 


2-80 


0140 


0-96 


1-63 


0245 


1-68 


2-86 


0145 


0-99 


1-69 


0250 


1-72 


2-92 


0150 


1-03 


1-75 


0255 


1-75 


2-98 


0155 


1-06 


1-81 


0260 


1-78 


3-03 


0160 


1-10 


1-87 


0265 


1-82 


3-09 


0165 


1-13 


1-93 


0270 


1-85 


3-15 


0170 


1-16 


1-98 


0275 


1-89 


3-21 


0175 


1-20 


2-04 


0280 


1-92 


3-27 


0180 


1-23 


2-10 


0285 


1-95 


3-33 


0185 


1-27 


2-16 


0290 


1-99 


3-39 


0190 


1-81 


2-22 


0295 


2-03 


3-45 


0195 


1-34 


2-28 


0300 


2-07 


3-51 


0200 


1-37 


2-33 









APPENDIX 



121 



S 



co <M CM CM CM cq cq 



O O O O Oi O 



CiGi 
OOOOOOOOOOOOOOOOOOOOOOGOCOCOOOOOCO1>.I>. 



s* 



opopoipoipoipopopoipppo 



si 



78 



OOOOOOOOCOOOOOOOGOOOOOOOOOOOCOOOOOOOOO 



O O T I T I <M (M CO CO 
CM CM <M <M <M (N (N (M 

ft M 

00 

fcc J, 

"^ 

-ft 

I 



3f ^S cqcNi-Hr-iTiT lOoooooidiCiCidioooboo 

io Ci O Ci O> Ci O C5 C5 Ci O Oi 00 OO 00 CO 00 OO 00 00 
^ o 

P. .go 

I'M 



122 CEMENT CHEMISTS 1 HANDBOOK 

(28A) TABLE FOR USE WITH SLATER'S 
CALCIMETER. 

ESTIMATION OF CaC0 3 IN LIMESTONE. 



Heading. 


Weight taken 
A 

CaC0 3 
As reading. 


Weight taken 
B 

(875 of A) 

CaCOs 


Weight taken 
C 
(75 of A) 

CaC0 3 


70-00 


_ 


80-00 


93-34 


70-25 





80-28 


93-67 


70-50 





80-57 


94-00 


70-75 





80-85 


9434 


7100 





81-14 


94-67 


71-25 





81-42 


95-00 


71-50 





81-71 


95-34 


71-75 





82-00 


95-67 


72-00 





82-28 


96-00 


72-25 





82-57 


96-34 


72-50 





82-85 


96-67 


72-75 





83-14 


97-00 


73-00 





83-42 


97-34 


73-25 





83-71 


97-67 


73-50 





84-00 


98-00 


73-75 





84-28 


98-34 


74-00 





8457 


98-67 


74-25 





84-85 


99-00 


74-50 





85-14 


99-34 


74-75 





85.42 


99-67 


75-00 





85-71 


100-00 


75-25 





86-00 




75-50 





86-28 




75-75 





8657 




76-00 





86-85 




76-25 





87-14 




76-50 





87-42 




76-75 





87-71 




77-00 





88-00 




77-25 





88-28 




77-50 





88-57 




77-75 





88-85 




78-00 





89-14 




78-25 





89-42 




78-50 





89-71 




78-75 





90-00 




79-00 





90-28 




7925 





90-57 




79-50 





90-85 




79-75 





91-14 




80-00 





91-42 





APPENDIX 123 

(29A) TABLE OF CORRECTIONS TO BE ADDED 
TO CALCIMETER READING FOR VARYING 
AMOUNTS OF PEAT IN SLURRY. 

RESULT = CALD. CaC0 3 (54). 



CALCIMETER READING. 


Excess 
" LOBS" 
over 
CO 2 


69-20 
to 
69-83 


69-88 
to 
70-51 


70-55 
to 
71-18 


71-23 
to 
71-86 


71-90 
to 
72-53 


72-58 
to 
73-21 


73-25 
to 
73-89 


73-92 
to 
74-55 


74-59 
to 

75-22 


75'27 
to 

75-92 


1-50 


1-06 


1-07 


1-08 


1-09 


1-10 


I'll 


1-12 


1-13 


1-14 


1-15 


1-60 


1-13 


1-14 


1-15 


1-16 


1-17 


1-18 


1-19 


1-20 


1-21 


1-22 


1-70 


1-20 


21 


1-23 


1-24 


1-25 


1-26 


1-27 


1-28 


29 


1-30 


1-80 


1-28 


-29 


1-30 


1-31 


1-33 


1-34 


1-35 


1-36 


37 


1-38 


1 90 


1-35 


36 


1-37 


1-39 


1-40 


1-41 


1-42 


43 


44 


1-45 


2-00 


T42 


43 


1-44 


1-46 


1-47 


1-49 


1-50 


52 


53 


1-54 


2-10 


1-49 


50 


1-51 


1-53 


1-54 


1-56 


1-57 


59 


60 


1-61 


2-20 


1-56 


58 


1-59 


1-61 


1-62 


1-64 


1-65 


67 


68 


1-69 


2-30 


1-63 


65 


1-66 


1-68 


1-69 


1-71 


1-73 


74 


76 


1-77 


2-40 


1-70 


72 


1-74 


1-76 


1-77 


1-79 


1-82 


83 


84 


1-85 


2-50 


1-78 


80 


1-82 


1-83 


1-85 


1-87 


1-89 


90 


92 


1-94 


2-60 


1-85 


87 


1-89 


1-90 


1-92 


1-94 


1-96 


97 


98 


1-99 


2-70 


1-93 


95 


1-97 


1-98 


1-99 


2-01 


2-03 


2-05 


2-07 


2-09 


2'8.) 


2-00 


2-02 


2'04 


2-05 


2-07 


2-09 


2-11 


2-13 


2-15 


2-17 


2-90 


2-08 


2-10 


2-12 


2-13 


2-15 


2-17 


2-19 


2-21 


2-23 


2-25 


3-00 


2-15 


2-17 


2-19 


ii-21 


2-23 


2-25 


2-27 


2-29 


2-31 


2-33 


3-10 


2-23 


2-25 


2-27 


2-29 


2-31 


2-33 


2-35 


2-37 


2-39 


2-41 


3-20 


2-30 


2-32 


234 


2-36 


2-39 


2-41 


2-43 


2-45 


2-47 


2-49 


3-30 


2-37 


2-39 


2-41 


2-43 


2-46 


2-48 


2-51 


2-53 


2-55 


2-57 


3-40 


2-44 


2-47 


2-49 


2-51 


2-53 


2-56 


2-59 


2-61 


2-63 


2-65 


3-50 


2-52 


2-55 


2-57 


2-59 


2-61 


2-64 


2-67 


2-69 


2-71 


2-73 


3-60 


2-60 


2-62 


2-65 


2-67 


2-69 


2-72 


2-75 


2-77 


2-79 


2-82 


3'70 


2-68 


2-70 


2-72 


2-74 


2-77 


2-80 


2-82 


2-85 


2-87 


2-90 


3-80 


2-75 


2-77 


2-80 


2-82 


2-85 


2-88 


2-90 


2-93 


2-95 


2-98 


390 


2-83 


2-85 


2-87 


2-90 


2-93 


2-96 


2-98 


3-01 


3-04 


3-06 


4-00 


2-90 


2-92 


2-95 


2-98 


3-01 


3-04 


3-06 


3-09 


3-11 


3-14 


4-10 


2-97 


2-99 


3-01 


3-04 


3-09 


3-12 


3-14 


3-17 


3-19 


3-22 


4-20 


3-04 


3-06 


3-09 


3-11 


3-17 


3-20 


3-22 


3-24 


3-27 


3-30 


4-30 


3-12 


3-14 


3-17 


3-19 


3-25 


3-28 


3-30 


3-32 


3-35 


3-38 


4-40 


3-20 


3-22 


3-25 


3-27 


3-33 


3-36 


3-38 


3-40 


3-42 


3-44 


4-50 


3-28 


3-30 


3-33 


3-35 


3-41 


3-43 


3-46 


3-48 


3-50 


3-52 



In the first column find the Excess " Loss on ignition " over C0 2 , then in a 
line with it under the given calcimeter reading will be found the figure to be 
added in order to obtain " n,i,,io*o,i nnn 



Calculated CaCO,.' 



124 



CEMENT CHEMISTS 1 HANDBOOK 



(30A) TABLE OF 
PRESSURE OF AQUEOUS VAPOUR. 



af 






a . 


oT 


a . 




a 


aT 


a 


Temperatur 
Degrees C. 


Pressure in n 
of mercurj 


Temperatur 
Degrees C. 


Pressure in n 
of mercury 


Temperatun 
Degrees C. 


Pressure in n 
of mercurj 


P 


Pressure in n 
of mercury 


Temperatur 
Degrees C. 


Pressure in n 
of mercury 


5-0 


6-5 


9-0 


8-6 


13-0 


11-2 


17-0 


14-4 


21-0 


18-5 


5-5 


6-8 


9-5 


8-9 


13-5 


11-5 


17-5 


14-9 


21-5 


19-1 


6-0 


7-0 


10-0 


9-2 


14-0 


11-9 


18-0 


15-4 


22-0 


19-7 


6-5 


7-2 


10-5 


9-5 


14-5 


12-3 


18-5 


15-8 


22-5 


20-3 


7-0 


7*5 


11-0 


9-8 


15-0 


12-7 


19-0 


16-3 


23-0 


20-9 


7-5 


7-8 


11-5 


10-1 


15 5 


13-1 


19-5 


16 9 


23-5 


21-5 


8-0 


8-0 


12-0 


10-5 


16-0 


13-5 


20-0 


17-4 


24-0 


22-2 


8-5 


8-3 


12-5 


10-8 


16-5 


14-0 


20-5 


17-9 


24-5 


22-9 



APPENDIX 



125 



(3lA) TEMPERATURE CORRECTION TABLE 



XO5O5O5OiO5 



'-ii I fM i I ^-H C<1 C<l C<l <M ' 



^^^^OOOOOQDicboil>'l^l^t~t-XXXXC5O5C5C5C5C>-* 
~f. XXXXXXXX XXXXXXXXX XXX X X X X X X_X_Oj_Ci_C5_O5 OS O> 

x :c x x x x x x x x x x x^ x x x x x x x x x -/ /. x x x x x x cy ?- 



COeO^'*-^Tt< > <*iOOOOO^OCDCDCOIr-l>'t^I>'t^XXXXXO5C:O5C5C; 
XXXXXXXXX XXX XX X XJX_X_XJXJJC_XJX>_X_XJX X_X_Op_00 OP_X_05_05 

X_X_X.X_X X X._X X XXXXXXXXXXXXX 



cococococo^fj<oooioor--t--t--t^r >> xxxxxo55O5Oi 

X^C X X_X X X X X X X X X X X X X X X X X X X X X X X f. X r. X X X X 

x x x~ ss c: c: si ci"o O~o~ o o < i 



X X X X X X X XXX X_Jc_X_XJX X X X X X_X X _X_X X X X X X X X X_X_X. 
t t'-t^t'-r^XXXXXCJCJCSCSC; O O OO-H-HI I^HI iC^C^C^e^C^COCOCOCOCO 

XXXXXXXX X XXXXXXXXX X X X_X X X XXXXXXXXX X 



__X.X_X__X_X_X.X XX X__X_X^X _X XXXXXXXXXXXXXXXXXX 

"^^^^^c^c^^cococococo^T^-rtiT^T^ooibiO'OOO?!; 
xxxxxxxxxxxxxxxxxxxxxxxxo 



X X X X X X X 



^^^C^<NC<ie<IC<ICOCOCOCOCO-^TfTt<-^'<*iOiOtOiCiOCDCDCDCDCOlr'I>l>l>l>' 

xxxxxxxxxxxxxxxxxxxx xxxxxxxxxxxxx 



XXXXXXXXXXXXXX 



eoco-^T^-^TtHT^ibibibibibcbcbocbot^t^t- 

X X X X X X X X X X X X X X X X X X X X 



OO X X X X* X X* X X X X X X X X X X 

gggrss 



H CO IO t** Oi f~H CO lO l^* O5 * 

- ocb^Dcboot- 

X X X X X X X 



xxxxxxxxxxxxxxxx x xaoxxxxxxxxx 

X X X X X~ X X QO X X OD QO 00 QD X X X X X X X X X X X X X X 



X X X X X X 



_x __x_x_x_x xx x xx x x "x x xx x x xxx xjc x 



cocoj<^t<<>>i< 

X X X X X X X X X X X _X X 



XXXXXXXXXXXX X XXXXXXXX 




126 



CEMENT CHEMISTS 1 HANDBOOK 



(32A) BAROMETRIC PRESSURE CORRECTION 



740.5 

Mm. 


742 

Mm. 


743 

Mm. 


744.5 

Mm. 


745.5 

Mm. 


747 

Mm. 


748 
Mm. 


749.5 
Mm. 


751 

Mm. 


752 

Mm. 


753 

Mm. 


754.5 

Mm. 


756 

Mm. 


757 

Mm. 


758 

Mm. 


760 

Mm. 


81-93 

82-21 


81-78|81-63 
82-0681-91 


81-49 

81-77 


81-35 
81-63 


81-2281-08 
81-5081-36 


80-94 
81-22 


80-8080-67 
81-0880-95 


80-53 

80-81 


80-39 
80-67 


80-26 
80-54 


80-12 
80-40 


79-99 
80-27 


79-80 
80-08 


82-4882-33 


82-18 


82-04 


81-90 


81-77 


81-63 


81-49 


81-35 


81-22 


81-08 


80-94 


80-81 


80-67 


80-53 


80-35 


82-76 


82-61 


82-46 


82-32 


82-18 


82-05 


81-91 


81-77 


81-6381-50 


81-36 


81-22 


81-09 


80-95 


80-82 


80-63 


83-04 


82-69 


82-74 


82-60 


82-46 


82-33 


82-19 


82-05 


81-9181-78 


81-64 


81-50 


81-37 


81-23 


81-10 


80-91 


83-32 


83-17 


83-02 


82-88 


82-74 


82-61 


82-47 


82-33 


82-1982-06 


81*92 


81-78 


81-65 


81-51 


81-38 


81-19 


83-60 


83-45 


83-30 


83-16 


83-02 


82-89 


82-75 


82-61 


82-4782-34 


82-20 


82-06 


81-93 


81-79 


81-66 


81-47 


83-8883-73 


83-58 


83-44 


83-30 


83-17 


83-03 


82-89 


82-75 


82-62 


82-48 


82-34 


82-21 


82-07 


81-94 


81-74 


84-15 


84-00 


83-85 


83-77 


83-57 


83-44 


83-36 


83-16 


83-02 


82-89 


82-75 


82-68 


82-48 


82-34 


82-21 


82-02 


84-43 


84-28 


84-13 


83-99 


83-85 


83-72 


83-58 


83-44 


83-30 


83-17 


83-03 


82-89 


82-76 


82-62 


82-49 


82-30 


84-72 


84-57 


84-42 


84-28 


84-14 


84-01 


83-87 


83-73 


83-59 


83-46 


83-32 


83-18 


83-05 


82-91 


82-78 


82-59 


85-00 


84-85 


84-70 


84-56 


84-42 


84-29 


84-15 


84-01 


83-87 


83-74 


83-60 


83-46 


83-33 


83-19 


83-06 


82-87 


85-28 


85-13 


84-98 


84-84 


84-70 


84-57 84-43 


84-29 


84-15 


84-02 


83-88 


83-74 


83-61 


83-47 


83-34 


83-15 


85-56 


85-41 


85-26 


85-12 


84-98 


84-8584-71 


84-57 


84-43 


84-30 


84-16 


84-02 


83-89 


83-75 


83-62 


83-43 


85-83 


85-68 


85-53 


85-39 


85-25 


85-1284-98 


84-84 


84-70 


84-57 


84-43 


84-29 


84-16 


84-02 


83-89 


83-70 


86-12 


85-97 


85-82 


85-76 


85-53 


85-40 85-2685-12 


84-98 


84-85 


84-71 


84-57 


84-44 


84-30 


84-17 


83-98 


86-40 


86-25 


86-10 


86-04 


85-81 


85-6885-5485-40 


85-26 


85-13 


84-99 


84-85 


84-72 


84-58 


84-45 


84-26 


86-68 


86-53 


86-38 


86-32 


86-09 


85-96 85-82 85-68 


85-54 


85-41 


85-27 


85-13 


85-00 


84-86 


84-73 


84-54 


86-96 


86-81 


86-66 


86-60 


86-37 


86-2486-1085-96 


85-82 


85-69 


85-55 


85-41 


85-28 


85-14 


85-01 


84-82 


87-2487-09 
87-5287-37 


86-94 

87-22 


86-88 
87-16 


86-65 
86-93 


86-52 86-38 86-24 
86-8086-6686-52 


86-10 
86-38 


85-97 
86-25 


85-83 
86-11 


85-79 
85-97 


85-56 

85-84 


85-42 
85-70 


85-29 
85-57 


85-10 
85-38 


87-80 

88-08 


87-6587-50 

87-9387-78 


87-44 
87-72 


87-21 

87-49 


87-08 86-94 86-80 

87-3687-2287-08 

1 


86-66 
86-94 


86-53 
86-81 


86-39 
86-67 


86-25 
86-53 


86-12 
86-40 


85-98 
86-26 


85-85 
86-13 


85-66 
85-94 



APPENDIX 



127 



BAROMETRIC PRESSURE CORRECTION 



CaCo 3 ! 762 
per cent. Mm. 


763 

Mm. 


764.5! 766 j 767 

Mm. Mm. Mm. 


768 
Mm. 


769.7 
Mm. 


771 

Mm. 


772.2773.5774.7 

Mm. Mm. j Mm. 


776 

Mm. 
78-12 
78*40 
78*67 
78*95 

TA.OQ 


777.2 

Mm. 

77*99 

78-27 
78-54 
78-82 

rrn.iA 


778.5 
Mm. 


779.7 

Mm. 


781 
Mm. 

77-53 
77-71 

78-08 
78*36 

TQ.A/1 


71-5079*67 
71-7579-95 
72.0080-22 
72-2580-50 

rro.en QA-TQ 


79*53 
79*81 
80*08 
80-36 

>. i . -i i 


79*39 
79*67 
79*94 
80*22 
QA.KA 


79*2679*12 
79*5479*40 
79*8179-67 
80*0979*95 

QA.OTQA.OQ 


78*99 
79*27 
79*53 
79*82 

QA.l A 


78*80 
79*08 
79*35 
79*63 

TA.m 


78*67 
78*95 
79*22 
79-50 

TA.TQ 


78*53 

78*81 
79*08 
79*36 

TA.fi/4 


78*3978*26 
78*67 78*54 
78*9478*81 

79*2279*09 

| 

TA-KA Tn-on 


77-80 
78-08 
78*35 
78*63 

TQ.A1 


77-61 
77-95 
78-22 
78-50 

170.170 



72*75 81 *06 80*92 80*78 80*65 80-51 80-38 80-19 80*06 79*92 79*78 79*65 79*52 79*38 79-19 79-06 78-92 



! 

73-00 81 -34 81 *20 81*06 80*93 80*79 80*66 80*47 80*34 80*20 80*06 79*93 79-7979-6679-47 79'34 



7 3-25 81 *62 81 *48 81 *34 81 *21 81 -07 80*94 80'75 80'62 80*48 80*34 80*21 80'07 79*94 79*75 79*62 



73-5081*8981-7581*61 



81 -48 81 *34 81 -21 81 "02 80*89 80*75 80'61 80*48 80*34 80*21 80*02 79*89 



75-OO 83-57 83*43 83-29 83*16 83*02 82*89 82*70 82*57,82*43 82*29 82*16 82*02 81 *89 



74-75 83-30 83*16 83-02 82-89 82-75 82*62 82*43 82*38 82*16 82*02 81*99 81-75 81-62 81-43 81*30 






73*75 82*17 82*03;81*8981*76 81*62 81*4981-30 81-17 81*03 80*89 80*76 ; 80*62 80*49 80*30 80*17 80 *03 
74'00j82*46 82*32i82*18 82*05 81 *91 81 '78 81 *59 81 '46 81 "32 81 *18 81 *05'80*91 80*78 80'59 80*46 80*32 
74-25 82*74 82*60 82*46 82*33 82*19 82*06 81 *87 81 -74 81*60,81*4681*33181 *19 81 *06 80*87 80-74 80 -60 
74-50 83*02 82-88 82*74 82*61 82*47 82*34 82*15 82*02 81'88 81 '74 81 "61 J81 -47 81-34 81'15 81-02 80*88 

l_^ . . .. . _ o ri r 



79*20 
79*48 
79*75 



75-25 83*85 83*71 83*57 83*44 83*30 83*17 82-9882-85 82-71 82*57 82*44 82*30 82*17!81-98 81'85 81'7 



75-50 84-13 83-99 83*85 83*72 83'58 83*45 83*26 83*13 82*99 82*85 82*72 82*58 82*45 82*26 82-13 

j 



1*7081*57 



81-94 

75-75!84*41 84*27 84*13 84*00 83'86 83*73 83'54 83*41 83*27 83*13 83*00 82*86 82*73 ; 82*54 82*41 82*2 

I I * 

76-00 84*69 84-55 84*41 84*28 84*14 84-01 183*82 83*69 83*55^3*41 83*28 83*14 83*01 82*82 82*69 82*5, 

76-25 84*97 84*83 ! 84*69 84*56 84*42 84*29 84*10 83*97j83*83 ( 83*69 SS-Se^^jSS^ 83*10 82*97 82*8 
76-50 85-25 85-1 184-97 84*84 84*70 84*57 84*38 84*25 84*11J83*97 83*84 83*70,83*57183*38 83-25 83*1 



81*16 
81*43 



I I 









76-75 85-53 85'39 85'25 85'12 84*98 84*85 84*66 84*53 84*49 84*25 84*12 83*98 83*85 83 -66 83'53 83'3 

II i i 

I I j 
77-00 85 *81|85*67 85-53 85*40 85-26 85*13;84*94 84*81 84*77,84*53 84*40 84*26 84*13 83*94183*81 83-6 



128 



CEMENT CHEMISTS 1 HANDBOOK 



o o o co o o 

CO 00 Ol O **" rH O 

o 



CO O 

C5 O 



CO 

w 

CO 



U 

s 



CO 
CO 



O 



Ol CO rH t^ <X> CO 

GO b- t^ Ol f- 00 

Ol O5 CC rH r O 

Ol CO ^O 



l 

I CO CO 



oo 01 o 

HH ~- I - 



bl 



rH O t^ <N O 
CO rH ^* 



E O O CO 

>^. 03 * 

O o co 01 
COS 



GO 



GO O 
CO rH 



CO 



p 

rH 6 



Ol Ol CO O C5 

^tl CO -TfH O5 O 



O 

O 



?c| 



5 



O^-a 



*ii 

ce S) d 

^J S-'l ' J 

lllJlll 

02 < pin hH i^ M "S 




APPENDIX 



129 



oc o ^ x 

o O 6 cr. 
II II II 7 




o-S 





u 
en 
D 

o 

K 
CJ 

U 



oc o 

o -? 
os o 



2 O 



5?, 



86 

IT 

el 



wu -^g 

^L- c c 

. 
l| 

yil 

SM^ 



11 



, 
2 



< o ^-i I 



I O QO 



* (M O "M 



I 



II! Hil 



3 o 



cj cj . 

IJtt 

S 02 *$ 



130 CEMENT CHEMISTS 1 HANDBOOK 



a 



o 01 o o GO o 



(M 



CO 



W HK SOS" 1 ^ 

<frl 
3 
w s 

s J 



*Sg 



H 



a *< ~* O 
2 Q 3 oo cs 



H O 
CM ^ 



O 



CO 

H 



<M O 



2 02 
hJ 



CO 



W 

2: >i 



; o to rH n <M 

TO cp p Ci 

O ^^-S ^ 



W 



O 

rH 
0, 



fa 3 



i<0 Or-oOrH 

<M T- CP 



o to o o to o t^ 

-tt^Nj C5 TOOl'qO<>l 

(f 1 O O CO rH O rH 

CM rH O 



O 

-4 

cu 



o 

CO 

CO 

r-1 
2 



TO O -H GO CO 
TO (>1 TO "^ O 

rH 4fl TO 



OQ .3 

05 S o^ 

s1^ 

J < & 03 
W ^ _CJ o 

FH F - 

6 fl o 
Q * 



o g 

bJO.2 



il 



i-< O < 

O f "3 

a ^ S S 

a as s J^ 



fa 
O 

CO 
CO 

rJ 



H as 
^5 

| 



TO 



rH rH rH r-l 



00 O (M h- 'M 

O O .Li Ci TO 



bDOi 

i J 



APPENDIX 



LLLON. 


_ o 
o o oo o : 

gp2| == 


= .= 


Is 

a 


rt? 

^S g.SJ 

Sill 


ill- 

SO ft 'S 


s 






a 
3 


?=-! 


25^ 










- s 


ll 


w 


I 






"S.S 












"""^ "** '^ " 


H 


p* 


O-H^^H _ 


M 




s ^ ^^ 2 


I J 


CO 


J o o cb >> *5 "S 


O '3 
O "- 1 


s S 




11 


\ 


3 




1^^^ 


Hi'" 


CO M 





z 

o 


3 1 F c i s 


|| 


- S 

?!l 


ll 


i i 


' " ,c 


9 l-sljf 


ill 1 1 

03 ^3 


III 


41 


S 


to 


J*i* 


sp-S 


5.S - 


5 I 


m 




^ s 


*+H ci 


B 


t+H 


H 












.. 


< 


E 

fee _ 


a: 

3 . 




*o 5 - 


* o 







i II 


1 bo 


S'^ p . 1 


ll 




^^ *" O ^ G o ^* r ^ 


O cS Z^ 


^ 


r 5 ^D b) ^* 


JH 3j* 


|H| 


* ^ r - 


'a C5 




tX; ^ S3 2 


3 -2 


(5 


g 


tc 




S ~ 1 




HH 

cu 


| 


*J 




=5 I ^ 


fil 


p* 


oo "3 ^ 


O 




I; s 


^5 3 S . 


f 1 


7* g >j tC.Ti ~ 


H2 


|?o^ 


is 72 *S 


P*3 ^ B 




^ s ^) ^y* .4^ .^ 5 fl 


^M r^ 


1 r-l 


^ " ^2 


^ "M -^ 


o 


JC 







" 


V3 3 CD 


CO 
Ul 


g 


' -S 




-+J 


P* 


s 

< 


|s=g| 7Z~ 


U5 > 5T 

? 13 o 


S 

S 

ll i 

1 


^ ^C 

3.3 *-' 

g-5 * 

8 1? 

s ^ 


2? 




S 


*"" -3 




5 


o 


RESULT OF / 


Chlorine as chlorides 
" Free " ammonia . 
"Albuminoid" amm 
Total solids . . . 
Colour of ditto . . 

Nitric acid as nitrates 
Equal to nitrogen . . 
Oxygen required to 
oxidise decompos- 


ing matter . . 
Sediment and micro- 
scopic results . . 


Colour of water . . 
Temporary hardness . 
Permanent 


-g 
o 


i 

3 
o 
/A 

s 

| 

5 



CEMENT CHEMISTS 1 HANDBOOK 



(34A) 
TABLE FOR USE WITH BLOUNT'S FLASK, 



SPECIFIC GRAVITY. USING 50 GRAMS OF 
CEMENT AND 50 c.c. OF OIL. 



Volume of oil 
displaced. 


Specific 
Gravity. 


Volume of Oil Specific 
displaced. Gravity. 


15-00 


3-333 


15-90 


3-145 


15-10 


3-312 


15-95 


3-135 


15-20 


3-290 


16-00 


3-125 


15-30 


3-268 


16-05 


3-115 


15-40 


3-246 


16-10 


3-105 


15-50 


3-225 


16-15 


3-095 


15-55 


3-215 


16-20 


3-086 


15-60 


3-205 


16-25 


3-077 


15-65 


3-195 


16-30 


3-067 


15-70 


3-185 


16-35 


3-058 


15-75 


3-175 


16-40 


3-049 


15-80 


3-165 


16-45 


3-039 


15-85 


3-155 


16-50 


3-030 



Sp. gr.= 



50 



c.c. displaced 



APPENDIX 133 

(3 5 A) Table for Use with Anderson's Specific Gravity 
Bottle using 150 grams of Cement and 200 c.c. of Oil. 



Displace- 
ment. 


Specific 
gravity. 


Displace- 
ment. 


Specific 
gravity. 


Displace- 
ment. 


Specific 
gravity. 


45-0 


3-333 


49-0 


3-061 


53-0 


2-830 


1 


3-326 


1 


3-055 


1. 


2-824 


"2 


3-319 


2 


3-049 


2 


2-820 


3 


3-311 


3 


3-043 


3 


2-814 


4 


3-304 


4 


3-046 


4 


2-809 


5 


3-297 


5 


3-030 


*i> 


2-804 


6 


3-289 


*6 


3-024 


6 


2-800 


7 


3-282 


7 


3-018 


7 


2-793 


8 


3-275 


8 


3-012 


8 


2-788 


9 


3-268 


9 


3-006 


9 


2-783 


40-0 


3-261 


oO'O 


3-000 


54-0 


2-777 


1 


3-254 


1 


2-994 


1 


2-773 


2 


3-247 


2 


2-988 


2 


2-768 


3 


3-240 


3 


2-982 


3 


2-762 


4 


3-233 


4 


2-976 


4 


2-757 


5 


3-226 


*5 


2-970 


*5 


2-752 


6 


3-219 


6 


2'964 


6 


2-747 


7 


3-212 


7 


2-959 


*7 


2-742 


8 


3-205 


8 


2-953 


8 


2-737 


9 


3-198 


9 


2-947 


9 


2-732 


47-0 


3-191 


51-0 


2-941 


55-0 


2-727 


1 


3-185 


1 


2-935 


1 


2-722 


"2 


3-178 


2 


2-930 


2 


2-718 


3 


3-171 


3 


2-924 


3 


2-712 


4 


3-165 


4 


2-918 


4 


2-708 


5 


3-158 


"5 


2-913 


*5 


2-703 


6 


3-151 


6 


2-907 


6 


2-698 


7 


3-145 


7 


2-901 


7 


2-693 


8 


3-138 


8 


2-896 


8 


2-688 


9 


3-132 


9 


2-890 


9 


2-683 


48-0 


3-125 


52-0 


2-885 


56-0 


2-078 


1 


3-119 


1 


2-879 


1 


2*674 


2 


3-112 


"2 


2-874 


2 


2-669 


9 


3-106 


3 


2-868 


3 


2-664 


4 


3-099 


4 


2-863 


4 


2-659 


5 


3-093 


*5 


2-857 


5 


2-654 


6 


3-086 


6 


2-852 


6 


2-650 


7 


3-080 


7 


2-846 


*7 


2-646 


8 


3-074 


8 


2-841 


8 


2-641 


9 


3-068 


9 


2-836 


9 


2-636 



Sp. gr. = 



150 



c.c. displaced. 



134 CEMENT CHEMISTS 1 HANDBOOK 



USEFUL DATA FOR TESTING-ROOM. 

For each neat briquette in British standard 
mould take 130 grams of neat cement, and gauge 
with correct proportions of water. 

26 '0 c.c. water used = 20 per cent. 

27-3 - 21 

28-6 - 22 

30-0 = 23 

31-2 = 24 

32-5 = 25 

For each sand briquette take 

37 grams of cement, 
111 ,, standard sand. 

10*5 c.c. water used = 7 per cent. 

^ 55 5 J ^ J 5 

13-5 - 9 
lo'O = 10 

For each Le Chatelier expansion test use 
50 grams of cement. 



APPENDIX 135 



To convert 

Lbs. per sq. inch into kilos per sq. centimetre 

x by '0703 

Kilos per sq. centimetre into Ibs. per sq. inch 

x by 14-223 

Holes per sq. centimetre into holes per sq. inch 

x by 6'45 

Holes per sq. inch into holes per sq. centimetre 

x by '155 

Grams into grains x by 15*43235 

Grains into grams x by '0648 

Degrees Centigrade into degrees Fahrenheit (F.) 

9 
x - and add 32. 

Fahrenheit into Centigrade (C.) 

5 
subtract 32 and x by <r. 



INDEX 



ALKALINE permanganate, 73 
Ammonium chloride, Standard, 75 
Apparatus required, 3 
Appendix, 107 
Aspirator, 17, 85 
Authors, consulted, 4 

BAMBER'S calcirneter, 48 

Bayley, 4 

Beringer, C. & J. J., 4 

Blount &; Stauger, 4 

Books consulted, 4 

British coals, Analyses of, 61 

CALCDIETERS, 44 

,, Bamber's, 48 

,, Slater's, 45 

Calculation of proportions, 39 

lime in clinker, 52 

Calorific power of fuel, 00 
Chemicals required, 2 
Clays for cement, 39 
Clowes & Coleman, 4 
Coal, Fineness of, 61 
Collection of samples fuel, 50 
gas, 84 

ru\v mate- 

rials, 5 

,, slurry,&c.,41 

water, 07 

Collins, W. D., 83 
' Colliery Guardian," 01 
Combustion in rotary kiln, 90 
Control of raw mixture, 53 
Copper chloride solution, 80 
Copper sulphate, pumice, 10 

DENNIS. 4 

Dreverhoff. Max, filter-paper. 15 

ECKEL, 4 

Elutriation, 24 

* Engineering Chemistry," 1 



Engineering Record," 83 
Equivalents, 2 

FILLING gas burette, 86 
Formulas, Calculation from, 39 
Fusion, 23 

GAS burette, Filling, 86 

HBMPEL, 4, 86 

Hem pel's apparatus, 86 

INDIGO, Solution of, 79 
Introduction, 1 
Iron, Estimation of, 28, 29 
pyrites in clay. 29 

KILN gas, 90 

LEWKOWITSCH on oils, 02 
Limestones for cement, 38 

MEADE, R. K. (Portland cement), 
by, 4, 51, 100 

XEILSON'S sulphur in coke, 05 
Sessler's reagent, 75 

ORSAT gas apparatus, 89 
Orton, 4, 90 

PHILLIP'S " Engineering Chemis- 
try," 1 

Potash for absorption, 80 
Pjrogallol for absorption, 80 

QUARTERING, 5 

RAW materials, calculation of pro- 
portion, 38 

Raw mixture, Control and alteration 
of, 53 

Reagents required, 



137 



138 



INDEX 



Keddrop's system, 1 
Redwood's viscosimeter, 63 

SAPONIFICATION equivalent, 66 

Separation of soda and potash. 32 

Shales for cement, 39 

Shinier crucible, 101 

Slurry. Dry standard, 44, 45 

Smith, Lawrence, 31 

Specific gravity, oils, 62 

Standard ammonium chloride, 7'> 
,, soap solution, 71 
potassium nitrate, 79 

,, permanganate, 

102 



Stanger and Blount, 4 
Strength of solutions, 1 

TAYLOR, 1 

Thermal units, 61 

Thompson, Lewis, calorimeter, 60 

VOLUMETRIC determination of lime, 

12 
Volumetric determination of lime, 

Rapid, 101 

WATER softening, 81 

, , Lime required, 83 



INDEX TO ANALYTICAL PROCESSES 



Analysis of Ash of coal 

Calcareous shale . . 

Loss on ignition 

Silica . 

Alumina and ferric oxide 

Liine and magnesia . 
Cement, Accurate . . 

Technical 

Loss on ignition 

Silica and insoluble . . 

Insoluble . 

Alumina and ferric oxide 

Lime . . . 



Magnesia . . 

Alkalies 

Sulphuric anhydride . . 
Sulphur as sulphide . 
Carbon dioxide 
Keene's 

Loss on ignition 

Silica and insoluble . 

Alumina and ferric oxide . 

Lime ,. 

Sulphuric anhydride . 
Chalk . . . .* . 

Moisture 

Loss on ignition 
Silica and insoluble . 
Alumina and iron oxide . 
Lime .... 
Calcium carbonate . 
Carbon dioxide 

Magnesia. . . . . 
Alkalies . .... 
Sulphates : . 

Clay . . . 

Moisture ..... 
Loss on ignition . . 

139 



Paragraph 


Page 


64 


59 




22 


16 


22 


17 


22 


17 


24 


17 


24 


117 


91 


123 


95 


130 


100 


117.123 


91,95 


127 


97 


118,124 


92,96 


119,120, 


92, 93, 


125, 132 


96, 101 


121,126 


93, 96, 97 


122 


94 


128 


98 


120 


99 


131 


100 


134 


102 


138 


103 


135 


102 


136 


102 


136 


102 


137 


103 


1 


6 


2,3 


6 


4 


7 


5,6 


.8,9 


7 


10 


8, 9, 10 


11 


9 


12 


14,15 


16,19 


11 


13 


12 


15 


13 


15 


18 


25 


18 


25 


28 


30 



140 INDEX TO ANALYTICAL PROCESSES 





Paragraph 


Tagc 


.A-llil! VSis of CljlY " COH^iM'H^cZ 






Silica and insoluble t 


li), 28 


26,28 


Sand . ...... 


18 


24 


Alumina and iron oxide .... 


19,24, 


26, 28, 29 




25, 20, 27 




In insoluble 


21 


27 


By fusion ..... 


22 


27 


Lime ....... 


19,24 


26, 28 


Magnesin 


19,24 


26, 28 


Alkalies ....... 


31 


31 


Sulphur ....... 


2!), 30 


30, 31 


Titanium oxide ..... 


20 


27 


Soluble chloride 


32 


33 


Coal 


i>7 


57 


Moisture . 


58 


57 


Sulphur ....... 


03 


59 


Ash 


59 


57 


Volatile matter 


oo 


57 


Fixed carbon 


61 


58 


Coke .... 


02 


58 


Coke 


05 


60 


Dolomite ....... 




21 


Gault clay ....... 


10,17 


22 


Gas, furnace, rotary kiln .... 




84 


Collection of samples .... 


101. 105 


S4, 85 


In Hempel apparatus .... 




86 


Carbon dioxide ..... 


110 


87 


Oxygen ... 


111 


88 


Carbon monoxide 


112 


88 


Nitrogen 


113 


89 


Combustible ...... 


114 


89 


In Orsat apparatus ..... 


115 


89 


Gypsum see Cement, Keenc's .... 


134 


102 


Keeue's cement 


134 


102 


Limestones see Chant 


1 


6 


Lime ........ 


139. 140 


103 


Lubricants 




61 


Loss or gain on exposure .... 


68 


62 


Specific gravity ..... 


69 


62 


Viscosity . 


78 


63 


Flash point ...... 


71 


64 


Free mineral acids 


72 


64 


Fatty acids 


73 


65 


fSeparation of fatty and mineral oils 


74 


65 


Magnesian limestones see Dolomite 




21 


Marl see Gault clay 


1 6-1 7 


22 


Natural cement rock 




34 


Plaster see Cement, Keene's .... 


134 


102 


Kaw materials see Limestone and Clay 




5 


Raw meals see Slurry . . . ' . 




41 


Scales, sandstones, slates .... 




34 


Slags 


33 


34 


Silica 


33 


34 


Alumina .... 


34, 35 


34, 35 


Iron oxide 


38 


35 



INDEX TO ANALYTICAL PROCESSES 141 





Paragraph 


Page 


A Y1 n 1 ITCI i fif Cl ^ rv y*^-. liZ^ntfrl 






-YlUll\fr]?? OI ol*lg;~~~CC//6cilt t'.C t'- 


36 


3.-. 


Lime and magnesia ..... 


37 


35 


Phosphorus ' 


39 


36 


Sulphur . 


40 


37 


Slurry . . ... 




41 


Obtaining samples- for .... 


42 


41,42 


Moisture 


41 


42 


Loss on ignition 


43 


42 


Silica, alumina and iron oxide, lime, mag- 






nesia, etc. . 


44 


42 


Calcium carbonate . . . ... 


47 


43 


On Slater's calcimeter 


50 


45 


On Bamber's calcimeter . 


50 


4s 


By standard acid . . . . 


52 


51 


By calculation . . .:-*-- i-. 


54 


52 


Lime calculated .... , a % , .. 


55 


52 


Organic matter 


45 


43 


Water, collection of samples for 


75 


67 


Colour, odour, reaction .... 


76 


(>~ 


Sediment and suspended matter 


77 


68 


Total solids 


78 


69 


Qual. and quan. anal, of . 


79 


69 


Chlorine as chlorides .... 


80 


70 




81 


71 


By standard soap .... 


82-85 


71,72 


Temporary . . . ' . 


85 


72 


Permanent . . . . . 


86 


72 


By standard acid . . . . f . , 


87,88 


73 


In a softened water .... 


89 


74 


Free ammonia . . : *V 


90,91.93 


75 


Albuminoid ammonia . . 


92,94 


75, 76 


Oxygen to oxidise . . . , 


95 


77 


Nitrates and nitrites . 


96, 97 


78, 79 


Poisonous metals . . 


98 


80 




INDEX TO APPENDIX 

Table rage 
1A. Calculations occurring during clay analysis .... 107 

2A. To ascertain proportions to obtain desired raw mixture . . 107 

3A. To produce mixture containing certain percentage of CaCO ; , . 109 

F ' \ Calculations occurring during slurry analysis .... 109 

6A. Directions for making up equivalent solutions, etc. . . 110-113 

7A. Preparation of normal sodium carbonate solution . . .113 

8A. Preparation of decinormal sodium carbonate solution . .113 

9A. Preparation of normal sulphuric acid solution . . . .113 

10A. Preparation of decinormal sulphuric acid solution . . .113 

HA. Preparation of normal hydrochloric acid solution . . . 114 

12A. Preparation of deciuormal hydrochloric acid solution . . .114 

13A. Preparation of normal sodium hydrate solution . . . .114 

14A. Preparation of decinormal sodium hydrate solution . . .114 

15 A. Preparation of normal potassium hydrate solution . . .114 

16A. Preparation of deciuormal potassium hydrate solution . .114 

17A. Preparation of decinormal potassium permanganate solution . 115 

ISA. Preparation of decinormal potassium bichromate solution . . 115 

Preparation of decinormal silver nitrate solution . . . .115 

19A. Preparation of litmus solution . . . . . . .116 

20 A. Preparation of methyl orange solution . . . . .110 

21 A. Preparation of phenolphthalein solution . . . . .116 

22A. Table of atomic weights . . . . .. . .116 

23A. Factors for use in analysis . . . . . . .117 

24A. Table for estimation of lime in cement . . . . .118 

25A. Table for estimation of magnesia in cement . . . .119 

26A. Table for estimation of sulphuric anhydride in cement . .120 

Tables for use with Slater's calcimeter .... 121-122 



29A. Table for correction of calcimeter reading ..... 122 

30A. Table of pressure of aqueous vapour . . . . . .124 

31A. Table for temperature correction for Bamber's calcimeter . . 125 
32A. Table for barometric correction for Bamber's calcimeter . . 126 
33A. Typical analyses, limestones, clays ..... . 128 

Typical analyses, shale, calcareous cla} r , slag, puxzolanic 

material .......... 129 

Typical analyses, raw meals, slurries, cements . . . .130 

Typical analyses, waters ........ 131 

34A. Table for use with Blount's specific gravity flask . . . 132 
35A. Table for use with Anderson's specinc gravity flask . . . 133 

Useful data for testing-room ...... 134.135 



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ANDREWS (L.), Electricity Control, 48 
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MUNRO(R. D.), Works by.. . . 32 
N A YLOR(W.), Trades' Waste, . . 76 
NICHOLSON (W.), Smoke Abatement, 76 
NORTH (S.), Oil Fuel, .... 61 
OPPENHEIMER (C.), Works by, 74,75 
OSMOND & STEAD, Micro. Analysis, 60 
PARK, (J.), Cyanide Process, . . 59 

Mining Geology, . ... 56 

PE ARC E (W.J.), Painting, . . . 80 
PETTIGREW (W. F.), Loco. Eng., . 30 
PHILLIPS & BAUERM AN, Metallurgy, 60 
POYNTINGJ& THOMSON, Physics, . 50 
PRAEGER (R. L.), Open Air Botany, . 85 
RANKINE'S Works, .... 35 
RAWSON, GARDNER, & LAYCOCK, 

Dictionary of Dyestuffs, . .82 

REDGRAVE (G. R.), Cements, . . 76 
REDWOOD ( Sir Boverton), Petroleum, 61 

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REED (Sir E. J.), Stability of Ships, . 37 
REID (Geo., M.D.), Sanitation, . . 78 
RICHMOND (H.D.), Works by, . 73 
RIEMER (J.), Shaft Sinking, . . 58 
ROBERTS -AUSTEN, Metallurgy, . 63 
ROBINSON (Prof.), Hydraulics, . . 36 
ROSE (T. K.), Gold, Metallurgy of, . 63 
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SEATON (A. E.), Marine Engineering, 44 
& ROUNTHWAITE, Marine 

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SHELTON (W. V.), Mechanic's Guide, 36 
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SMITH, (W. J.), Shipmaster's Med. Help, 4S 
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STRICKLAND F.), Petrol Motors, . 33 
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TRAILL (T. W.), Boilers, . 29 

TROTMAN (S. R.), Leather, . . 81 
TURNER (Thos.), Iron, Metallurgy of, 65 

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WALTON (T.), Works by, . . 38, 44 
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WELLS (S. H.), Engineering Drawing, 32 
WIGLEY (T. B.), Jeweller's Art, . 68 
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WOOD (Francis), Sanitary Engineering, 78 
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WRIGHT (Dr. A.). Oils and Fats, . 71 
ZERR & RUBENKAMP, Col. Manuf., 80 



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The Engine Accessories. Electrical Ignition. The Chassis and Driving 
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By F. STRICKLAND. 

GENERAL CONTENTS. PART I. : ENGINES. Historical. Power Required. General 
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Pipe Arrangements. Silencers. Engine Control, Balancing. Motor Cycle Engines. 
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HYDRAULIC POWER 



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BY 

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CONTENTS Discharge through Orifices. Flow of Water through Pipes. Accumulators. 
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BY HENRY DAYEY, 

Member of the Institution of Civil Engineers, Member of the Institution of 
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CONTENTS Early History of Pumping Engines Steam Pumping Engines 
Pumps and Pump Valves General Principles of Non-Rotative Pumping 
Engines The Cornish Engine, Simple and Compound Types of Mining 
Engines Pit Work Shaft Sinking Hydraulic Transmission of Power in 
Mines Electric Transmission of Power Valve Gears of Pumping Engines 
W ater Pressure Pumping Engines Water Works Engines Pumping 
Engine Economy and Trials of Pumping Machinery Centrifugal and other 
Low-Lift Pumps Hydraulic Rams, Pumping Mains, &c. INDEX. 

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STUDY." The Engineer. 

"Undoubtedly THE BEST AND MOST PRACTICAL TREATISE on Pumping Machinery THAT HAS 
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NAVAL ARCHITECTURE. 37 



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Geometry of a Ship's Form. Description and Instances of Ship's Forms. Description 
of Types of Ships. PART II. : Calculation of Displacement, Centre of Buoyancy and 
Areas. Metacentres. Trim. Coefficients and Standardising. Results of Ship Calcula- 
tions. Instruments Used to Determine Areas, Moments, and Moments of Inertia of 
Plane Curves. Cargo Capacities, Effects on Draught, Trim, and Initial Stability due 
to Flooding Compartments. Tonnage. Freeboard. Launching. Application of the 
Integraph to Ship Calculations.^Straining due to Unequal Longitudinal Distribution 
of Weight and Buoyancy. Consideration of Stresses in a Girder. Application of Stress 
Formulae to the Section of a Ship. Shearing Forces and Bending Moments on a Ship 
amongst Waves. Stresses on the Structure when Inclined to the Upright or to the 
Line of Advance of the Waves. Distribution of Pressure on the Keel Blocks of a 
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LECTURES ON THE MARINE STEAM TURBINE. 

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THE STABILITY OF SHIPS. 

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CNIGHT OF THE IMPERIAL ORDERS OP ST. STANILAUS OF RUSSIA ; FRANCIS JOSKPH OF 

AUSTRIA ; MKDJ1DIB OF TURKEY ; AND RISING SUN OF JAPAN ; VICB- 

PRESIDENT OF THK INSTITUTION OF NAVAL ARCHITECTS. 



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FOURTH EDITION. Illustrated with Plates, Numerous Diagrams, and 
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STEEL SHI PS: 

THEIR CONSTRUCTION AND MAINTENANCE. 

A Manual for Shipbuilders, Ship Superintendents, Students, 

and Marine Engineers. 

BY THOMAS WALTON, NAVAL ARCHITECT, 

AUTHOR OF "KNOW YOUR OWN SHIP." 

CONTENTS. I. Manufacture of Cast Iron, Wrought Iron, and Steel. Com- 
position of Iron and Steel, Quality, Strength, Tests, &c. II. Classification of 
Steel Ships, III. Considerations in making choice of Type of Vessel. Framing 
of Ships. FV. Strains experienced by Ships. Methods of Computing and 
Comparing Strengths of Ships. V. Construction of Ships. Alternative Modes 
of Construction. Types of Vessels. Turret, Self Trimming, and Trunk 
Steamers, &c. Rivets and Bivetting, Workmanship. VI. Pumping Arrange- 
ments. VII. Maintenance. Prevention of Deterioration in the Hulls of 
Ships, Cement, Paint, &c. INDEX. 

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PRESENT-DAY SHIPBUILDING. 

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Plating, Rivetting, Stem Frames, Twin-Screw Arrangements, Water 
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KNOW YOUR OWN SHIR 

BY THOMAS WALTON, NAVAL ARCHITECT. 
Specially arranged to suit the requirements of Ships' Officers, Shipowners, 

Superintendents, Draughtsmen, Engineers, and Others, 
CONTINTS. Displacement and Deadweight. Moments. Buoyancy. Strain. 
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Admission of Water into Ship. Trim Tonnage. Freeboard (Load-line). Calculations. 
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NAUTICAL WORKS. 39 



GRIFFIN'S NAUTICAL SERIES. 

EDITED BY EDW. BLACKMORE, 

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2 



40 CHARLES GRIFFIN & CO.'S PUBLICATIONS. 

GRIFFIN'S NAUTICAL SERIES. 

Introductory Volume. Price 8s. 6d. 
T ZEilE 

British Mercantile Marine. 

BY EDWARD BLACKMORE, 

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MEMBER OF THE INSTITUTION OF ENGINEERS AND SHIPBUILDERS 

IN SCOTLAND; EDITOR OF GRIFFIN'S "NAUTICAL SERIES." 

GENERAL CONTENTS. HISTORICAL : From Early Times to 1486 Progress 
onder Henry VIII. To Death of Mary During Elizabeth's Reign Up to 
the Reign of William III The 18th and 19th Centuries Institution of 
Examinations Rise and Progress of Steam Propulsion Development of 
Free Trade Shipping Legislation, 1862 to 1875 " Locksley Hall" Case- 
Shipmasters' Societies Loading of Ships Shipping Legislation, 1884 to 1894 
Statistics of Shipping. THE PERSONNEL : Shipowners Officers Mariners 
Duties and Present Position. EDUCATION : A Seaman's Education : what it 
should be Present Means of Education Hints. DISCIPLINE AND DUTY 
Postscript The Serious Decrease in the Number of British Seamen, a Matter 
demanding the Attention of the Nation. 

k INTERESTING and INSTRUCTIVE . . . may be read WITH PROFIT and ENJOYMENT."- 

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A XMUUEYTCJAJL, OF 

ELEMENTARY SEAMANSHIP. 

BY 
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YOUNGER BROTHER OF THE TRINITY HOUSE. 

With Frontispiece, Numerous Plates (Two in Colours), and Illustration! 

in the Text. 

GENERAL CONTENTS. The Building of a Ship; Parts of Hull, Masts, 
Ac. Ropes, Knots, Splicing, &c. Gear, Lead and Log, &c. Rigging, 
Anchors Sailmaking The Sails, &c. Handling of Boats under Sail 
Signals and Signalling Rule of the Road Keeping and Relieving Watch 
Points of Etiquette Glossary of Sea Terms and Phrases Index. 

** The volume contains the NEW RULES OF THE ROAD. 

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Although intended for those who are to become Officers of the Merchant Navy, it will be 
found useful by ALL YACHTSMEN." A thenmtm. 

** For complete List of GRIFFIN'S NAUTICAL SERIES, see p. 39. 

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NAUTICAL WORKS. 41 

GRIFFIN'S NAUTICAL SERIES. 

SECOND EDITION, Revised and Illustrated. Price 8s. 6d. 

NAVIGATION: 

PRACTICAL ANI> THEORETICAL. 

BY DAVID WILSON-BARKER, R.N.R., F.R.S.E., <fcc., <fco., 

AND 

WILLIAM ALLINGHAM, 

FIKST-CLASS HONOURS, NAVIGATION, SCIENCE AND ART DEPARTMENT. 

TRflitb Numerous ^lustrations anfc Bjaminatfon Gluestions, 

GENERAL CONTENTS. Definitions Latitude and Longitude Instruments 
of Navigation Correction of Courses Plane Sailing Traverse Sailing Day's 
Work Parallel Sailing Middle Latitude Sailing Mercator's Chart 
Mercator Sailing Current Sailing Position by Bearings Great Circle Sailing 
The Tides Questions Appendix : Compass Error Numerous Useful Hints 
&c. Index. 

" PRECISELY the kind of work required for the New Certificates of competency in grade* 
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" A CAPITAL LITTLE BOOK . . . specially adapted to the New Examinations. The 
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MARINE METEOROLOGY, 

FOE OFFICERS OF THE MERCHANT NAVY. 
BY WILLIAM ALLINGHAM, 

Joint Author of "Navigation, Theoretical and Practical." 

With numerous Plates, Maps, Diagrams, and Illustrations, and a facsimile 
Reproduction of a Page from an actual Meteorological Log-Book. 

SUMMARY OF CONTENTS. 

INTRODUCTORY. Instruments Used at Sea for Meteorological Purposes. Meteoro- 
logical Log-Books. Atmospheric Pressure. Air Temperatures. Sea Temperatures.- 
Winds. Wind Force Scales. History of the Law of Storms. Hurricanes, Seasons, and 
Storm Tracks. Solution of the Cyclone Problem. Ocean Currents. Icebergs. Syn- 
chronous Charts. Dew, Mists, Fogs, and Haze. Clouds. Rain, Snow, and Hail. 
Mirage, Rainbows, Coronas, Halos, and Meteors. Lightning, Corposants, and Auroras. 
QUESTIONS. APPENDIX. INDEX. 

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%* For Complete List of GRIFFIN'S NAUTICAL SERIES, see p. 39. 
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43 VHARLB* GRIFFIN A OO.'S PUBLICATION*. 

GRIFFINS NAUTICAL SERIES. 

THIRD EDITION, REVISED. With Numerous Illustrations. Price 3s. 6d. 

Practical Mechanics: 

Applied to the Requirements of the Sailor. 
BY THOS. MACKENZIE, 

Master Mariner, F.R.A.S. 

GENERAL CONTENTS. Resolution and Composition of Forces Work done 
by Machines and Living Agents The Mechanical Powers: The Lever; 
Derricks as Bent Levers The Wheel and Axle : Windlass ; Ship's Capstan ; 
Crab Winch Tackles : the "Old Man" The Inclined Plane; the Screw 
The Centre of Gravity of a Ship and Cargo Relative Strength of Rope : 
Steel Wire, Manilla, Hemp, Coir Derricks and Shears Calculation of the 
Cross-breaking Strain of Fir Spar Centre of Effort of Sails Hydrostatics : 
the Diving-bell ; Stability of Floating Bodies ; the Ship's Pump, &c. 

" THIS EXCELLENT BOOK . . . contains a LARGE AMOUNT of information. " 
Nature. 

" WELL WORTH the money . . . will be found EXCEEDINGLY HELPFUL." 
Shipping World. 

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CAPTAIN MACKENZIE'S ' PRACTICAL MECHANICS.' Notwithstanding my many 
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Mine Air, Investigation of, FOSTER AND HALDANE, . 54 

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DR. J. GROSSMANN, . 46 
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PROF. OASTELI/-EVANS, . 79 

H. D. RICHMOND, . 73 

E. F. WlLLOUGHBY, . 73 

C. A. MITCHELL, . 74 

DR. G. REID, . . 78 

F. WOOD, ... 78 
J. W. HARRISON, . 78 
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J. CLARK, . . . 73 

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DR. W. J. SYKES, . 75 

W. NAYLOR, . . 76 

WM. NICHOLSON, . 76 

G. R. REDGRAVE, . 76 
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DR. SCHWARTZ, . 

SIR BOVERTON REDWOOD, 
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THOS. LAMBERT, . 
R. S. TROTMAN, . 
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ARCHBUTT AND DEELEY, 
DR. CARL O. WEBER,. 
G. H. HURST, . 



W. J. PEARCE, . 
KNECHT AND RAWSON, . 
RAWSON AND GARDNER, 
CAIN AND THORPE, 
H. R. CARTER, . 
SEYMOUR ROTHWELL, . 
W. I. HANNAN, . 
G. H. HURST, 
GEO. DUERR, 



77 
61 
61 
81 
81 
81 
81 
71 
32 
81 
80 
80 
80 
82 
82 
82 
83 
83 
83 
84 
84 



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GLUE, GELATINE, 

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2 OHARLES GRIFFIN cfe CO:S PUBLICATIONS. 

THE TEXTILE JLJSTI* 



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And RICHARD LOEWENTHAL, Ph.D. 

GENERAL CONTENTS. Chemical Technology of the Textile Fabrics- 
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ASSISTED BY WILLIAM TURNBULL 

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86 CHARLES GRIFFIN <fe CO. 'S PUBLICATIONS. 

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